CN117551303A - Novel light-weight water sports board HEM molding material and molding process - Google Patents
Novel light-weight water sports board HEM molding material and molding process Download PDFInfo
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- CN117551303A CN117551303A CN202310057110.0A CN202310057110A CN117551303A CN 117551303 A CN117551303 A CN 117551303A CN 202310057110 A CN202310057110 A CN 202310057110A CN 117551303 A CN117551303 A CN 117551303A
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- water sports
- sports board
- foaming
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- KDQTUCKOAOGTLT-UHFFFAOYSA-N 3-[3-(dimethylcarbamoylamino)-4-methylphenyl]-1,1-dimethylurea Chemical compound CN(C)C(=O)NC1=CC=C(C)C(NC(=O)N(C)C)=C1 KDQTUCKOAOGTLT-UHFFFAOYSA-N 0.000 claims description 5
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- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 claims description 3
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 claims description 3
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 101150041750 Surf4 gene Proteins 0.000 description 1
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Classifications
-
- 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
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/02—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles for articles of definite length, i.e. discrete articles
- B29C44/12—Incorporating or moulding on preformed parts, e.g. inserts or reinforcements
-
- 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
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
- B29C44/60—Measuring, controlling or regulating
-
- 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
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/68—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts by incorporating or moulding on preformed parts, e.g. inserts or layers, e.g. foam blocks
- B29C70/681—Component parts, details or accessories; Auxiliary operations
- B29C70/682—Preformed parts characterised by their structure, e.g. form
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/32—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof from compositions containing microballoons, e.g. syntactic foams
-
- 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
- B29L2031/00—Other particular articles
- B29L2031/52—Sports equipment ; Games; Articles for amusement; Toys
- B29L2031/5272—Surf boards
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2363/02—Polyglycidyl ethers of bis-phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2463/02—Polyglycidyl ethers of bis-phenols
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
A novel lightweight water sports board HEM molding material is obtained by the following method: preparing hydrophobic liquid or colloidal organosilicon modified epoxy polymer by using tetramethyl cyclotetrasiloxane, allyl glycidyl ether and styrene; 50-80 parts of epoxy resin, 5-10 parts of the organosilicon modified epoxy polymer and reactive epoxy dilution are utilized5-10 parts of agent and amino-terminated polyether for polyether modification; further emulsifying; adding water, dicyandiamide, an accelerator and a foaming agent into the emulsion to prepare a coating foaming material; coating and drying to obtain epoxy expansion core material EEC, its expansion ratio is 50-150 times, and density of foaming core material obtained after thermal expansion is 0.01-0.05g/cm 3 . The thermal expansion compression molding HEM technology is applied to compression molding of carbon fibers of the water sports board, has low density and controllable density, and can resist seawater adsorption and insolation. High forming efficiency, good quality and reduced raw material consumption.
Description
Technical Field
The invention relates to the field of manufacturing of lightweight water sports boards, in particular to a novel lightweight water sports board HEM molding material and a molding process thereof.
Background
Surfboards are generally constructed from an inner core and an outer cladding of fibrous layers. The inner core of the original surfboard is made of wood and is heavier. Because of the need for weight reduction, the current mainstream surfboards mostly use high density polystyrene Expanded Polystyrene (EPS) and polyurethane Polyurethane (PU). The core density is typically less than 0.025g/cm 3 While these materials tend to be difficult to withstand the challenges of conventional carbon fiber compression molding temperatures, which are typically 100-160 ℃ for 30-120 minutes, given that the core material may not decompose or expand or shrink during the temperatures and time periods described above, the appearance of the fibrous product is difficult to fill. In addition, no matter whether the water sports are performed in sea water or fresh water, if the surfboard surface layer is damaged and the core material absorbs water, weight is increased easily, ageing is accelerated, and the problem of bulge deformation or layering cracking easily occurs when the sun exposure temperature is increased.
The high-density polystyrene EPS foam is light in weight, good in strength and recyclable, is an environment-friendly material, is not suitable for a middle-low temperature molding process exceeding 100 ℃ because the EPS is subjected to volume shrinkage at a temperature exceeding 90 ℃, is only suitable for a hand lay-up fiber cloth covering process, cannot overcome all defects of the hand lay-up process, such as severe environment caused by volatile smell in hand lay-up resin, uncontrollable difference of product weight and size caused by manual production of workers, and needs long-time curing of the resin, so that the production efficiency is low.
Polyurethane PU foaming is an artificially synthesized high polymer foaming material, has good flexibility and good compression deformation resistance. However, the production of this material is not environmentally friendly, and the core material of the specific shape of the surfboard is obtained by CNC cutting and repeated sanding and finishing, resulting in a large amount of scrap that is difficult to recycle. Although the PU material is very durable in conventional environments, if the outer wrapped fibrous layer is damaged by trauma or rupture, the PU board core absorbs water and rapidly ages, causing the foam to rupture and become brittle. And the compression properties of PU are relatively poor, and when receiving small area impact, the core material is easily dented or crushed to cause irreversible damage.
A Polymethacrylimide foam (PMI) which is a cross-linked rigid structural foam material and has a 100% closed cell structure, and the uniformly cross-linked cell wall structure can endow the foam material with outstanding structural stability and excellent mechanical properties. CNC processing is necessary to be carried out on the core material, waste of leftover materials in the cutting process is caused, and the common waste rate is 30% -50%. The lower limit of the conventional density of the material is 0.025g/cm 3 Bottlenecks can occur if application scenarios of smaller densities are encountered. The carbon fiber prepreg as the core material and the outer layer is combined to ensure that interlayer combination is firm, a gluing process is added on the surface of the PMI core material, so that the efficiency is reduced, the weight is increased, and the cost is increased. In addition, since the foamed material is a rigid foam, the toughness and resilience are extremely poor, and when a small area impact is encountered, the core material is irreversibly damaged upon sagging or crushing.
In the molding process, the high-density polystyrene Expanded Polystyrene (EPS), polyurethane Polyurethane (PU) and polymethacrylimide foam (PMI) core materials are mainly adoptedCNC processing, fresh compression molding process. Patent CN103146216A discloses a high-energy adhesive product, a preparation method and application thereof. The high-energy adhesive product comprises the following components in parts by weight: 15-25 parts of thermoplastic rubber; 10-25 parts of ethyl acetate; 6-20 parts of foaming agent; 30-60 parts of butanone; 0.5-3 parts of plasticizer; 0.5 to 2.5 portions of anti-aging agent; 0.5-2% of stearic acid; 2-3.5 parts of cross-linking agent; 3-10 parts of polyester fiber. Is a chemical foaming material of thermoplastic rubber, and is difficult to realize the density lower than 0.025g/cm 3 The organic solvents used in the preparation process are also unfavorable for environmental protection and ensuring the healthy operation of staff in the production process.
Patent CN107089017a discloses a thermal expansion process of a high-energy glue molding fiber composite product. Cutting the fiber composite cloth and the high-energy adhesive according to the structural design specification and size, and finishing for later use; according to the mechanical structure design requirement, arranging and layering the fiber composite material cloth, and coating the fiber composite material cloth outside the high-energy adhesive to obtain a rolled product; preheating the obtained rolled product on a heating table at the temperature of between room temperature and 80 ℃ for 3 to 60 minutes, extruding as far as possible to remove interlayer gas, smoothing the pressure, then placing the product in a preforming die, and preforming according to the shape designed by the preforming die to obtain a preformed product; placing the obtained preformed product into a preheating oven at 35-75 ℃ for preheating for 3-60 min, taking out, placing into a forming die, and closing the die and tightly; the die is sent into a hot-press forming table, the high-energy adhesive is expanded and then is not contracted or is expanded and then contracted firstly under the action of a heating program, and the product forming is completed; and (3) conveying the molded die into a cooling table for cooling, conveying the cooled die into a demolding table, and opening the die to take out the product. The high-energy glue and the fiber composite cloth are subjected to expansion curing molding at one time, the implicit assumption of the process is only suitable for products with relatively thin thickness, if the problem that the curing of the prepreg and the expansion of the high-energy glue are asynchronous occurs when the products with the thickness exceeding 1cm are encountered, the high temperature of the mold can act on the closely attached fiber prepreg first to cause the prepreg to be cured quickly, and once the prepreg is cured first, the thermal expansion of the internal high-energy glue is limited, the foam expansion is insufficient, and the appearance of the products is not full enough.
Disclosure of Invention
The invention aims to solve the technical problem of providing a novel thermal expansion compression molding process HEM material which is suitable for carbon fiber compression molding, low in density, controllable in density, capable of resisting seawater adsorption and resisting insolation and a novel lightweight water sports board and a molding process thereof.
In order to solve the technical problems, the invention provides a novel light-weight water sports board HEM molding material, which is characterized by being prepared through the following steps:
step 1, preparing an organosilicon modified epoxy polymer: preparing a hydrophobic organosilicon modified epoxy polymer, siEP for short, by using tetramethyl cyclotetrasiloxane, allyl glycidyl ether and styrene;
step 2, preparing an organosilicon polyether modified epoxy polymer, siEEP for short, by using the following components in proportion:
1) 50-80 parts by weight of epoxy resin, EP for short,
2) The organosilicon modified epoxy polymer SiEP obtained in the step 1 is 5-10 parts by weight,
3) Epoxy reactive diluent, ED for short, 5-10 weight portions,
4) The mole number of N-H bonds contained in the amino-terminated polyether, PEA for short, is 0.2-0.5 times of the mole number of epoxy groups in the system;
step 3, adding the organosilicon polyether modified epoxy polymer SiEEP obtained in the step 2 into a solvent, emulsifying and diluting to obtain an organosilicon polyether modified epoxy emulsion, namely AQ-SiEEP; the formula adopted is as follows: the organosilicon polyether modified epoxy polymer SiEEP obtained in the step 2 is 100 weight parts, the cosolvent is 10-20 weight parts, and the main solvent is 60-100 weight parts;
Step 4, preparing a coating foaming material: the composite material is prepared by mixing the following components in proportion:
1) 50-70 parts by weight of organosilicon polyether modified epoxy emulsifier AQ-SiEEP,
2) 0 to 30 parts by weight of water,
3) The dicyandiamide DICY dosage is multiplied by the active hydrogen equivalent according to 0.9 to 1.0 times of the epoxy mole number of the organosilicon polyether modified epoxy emulsion AQ-SiEEP,
4) The usage amount of the accelerator is 0.5-1.5 times of the dicyandiamide DICY feeding weight,
5) 50-100 parts by weight of foaming agent;
step 5, preparing an epoxy expansion core material, namely EEC: coating the coating foaming material obtained in the step 4 on release paper, and drying to obtain an epoxy expansion core material EEC which can be peeled from the release paper, wherein the foaming multiplying power range of the epoxy expansion core material EEC is 50-150 times, and the density range of the foaming core material obtained after thermal expansion is 0.01-0.05g/cm 3 。
As a further preferable scheme, in the step 1, the molar ratio of the tetramethyl cyclotetrasiloxane, the allyl glycidyl ether and the styrene is 1:2:2; the preparation process comprises the following steps: adding tetramethyl cyclotetrasiloxane into a reaction kettle protected by inert gas, maintaining the temperature at 80 ℃, adding a mixture of 25% allyl glycidyl ether and 25% styrene under stirring at 500rpm, dropwise adding 20-60ppm of platinum catalyst with CAS number of 68478-92-2, maintaining stirring at 500rpm for 10min, dropwise adding the rest mixture of 75% allyl glycidyl ether AGE and 75% styrene ST, maintaining the temperature range of a dripping acceleration maintaining system in the process at 80-90 ℃, maintaining stirring for 4 hours after the dripping is completed, then heating to 120 ℃, removing the low-boiling point solvent under reduced pressure, and obtaining transparent liquid by discharging, wherein the absolute pressure is 10-20 KPa.
The SiEP obtained in the step 1 comprises two isomers with the following structural formula:
in the step 2, the epoxy resin is one or a combination of any two or more of epoxy resin E-06, epoxy resin E-12, epoxy resin E-20, epoxy resin E-44 and epoxy resin E-51; the epoxy reactive diluent is one or any two or more of benzyl glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, diglycidyl ether, 1, 6-hexanediol diglycidyl ether and polypropylene glycol diglycidyl ether; the amino-terminated polyether is one or a combination of any two or more of polyoxypropylene diamine D230, polyoxypropylene diamine D400, polyoxyethylene diamine ED600 and polyoxyethylene diamine ED 900.
The preparation process in the step 2 comprises the following steps: and (2) weighing epoxy resin EP according to a proportion, adding the organosilicon modified epoxy polymer SiEP obtained in the step (1) and an epoxy reactive diluent ED into a reaction kettle, maintaining the temperature at 70 ℃, stirring and mixing for 2-4 hours at 300-900rpm, adding amino-terminated polyether PEA according to the calculated amount of the materials, stirring and mixing for 1-2 hours at 300-900rpm, sealing at room temperature, and standing for more than 12 hours for standby, thereby obtaining the organosilicon polyether modified epoxy polymer SiEEP.
The main solvent in the step 3 is water; the cosolvent is one or any two or more than two of isopropanol, ethylene glycol butyl ether, ethylene glycol, propylene glycol methyl ether and dipropylene glycol butyl ether.
The specific implementation method of the step 3 is as follows: and (2) weighing the organosilicon polyether modified epoxy polymer SiEEP and the cosolvent obtained in the step (2) according to the proportion, sequentially adding the organosilicon polyether modified epoxy polymer SiEEP and the cosolvent into an emulsifying device, heating to 80 ℃, uniformly stirring at 900-1000rpm for 0.5 hours, cooling to 60 ℃, dropwise adding the main solvent while stirring at 3000rpm within 1.5 hours, maintaining high-speed shearing and emulsifying for 1 hour, cooling to 40 ℃, and stirring at 3000rpm for 1 hour to obtain the organosilicon polyether modified epoxy emulsion AQ-SiEEP.
In the step 4, the accelerator is preferably an organic urea accelerator, 1' - (4-methyl-m-phenylene) bis (3, 3-dimethylurea) having a CAS of 17526-94-2.
In the step 4, the foaming agent is thermal expansion microspheres; the foaming agent is selected from 551DU40, 461DU20, 051DU40, 920DU20, 920DU40 of NOURYON; or F-48D, F-50D, F-65D, MSH-340, MSH-550, F-100MD, F-78KD, F-82D of MATSUMOTO; or SEKISUI EHM204, EHM302, EM303, EM406, EML 101.
The EEC coating of the epoxy expansion core material obtained in the step 5 has a square gram weight of 100-300g/m 2 。
Meanwhile, the invention also provides a forming process for manufacturing the novel lightweight water sports board HEM by using the material, which is characterized by comprising the following steps of:
1) The volume of the foaming cavity is multiplied by the expected density of the core material to be 0.01-0.05g/cm according to the size of the foaming mould manufactured by the design size of the water sports board 3 Calculating the weight of EEC of the injected epoxy expansion core material; weighing an epoxy expansion core material EEC with corresponding weight, putting the EEC into the foaming mold, closing the mold and effectively locking the mold;
2) Transferring the foaming mould to a platen of a hot press to perform hot-press foaming expansion, and then performing cold pressing and cooling to obtain a foaming core material of the water sports board;
3) Wrapping fiber prepreg outside the foam core material of the water sports board to obtain a prepreg inclusion;
4) And (3) placing the prepreg inclusion into a forming die of the motion plate, hot-pressing on a platen of a hot press, and then cold-pressing and cooling to obtain the crude blank of the water motion plate.
As an important property obtained by the invention, the water absorption of the crude embryo of the water sports board is 20g-80g.
The preferred specific method of the step 2) is as follows: the foaming mould is transferred to a platen of a hot press, the platen of the hot press is connected with a heating device in advance, the temperature of the platen is maintained at 120-160 ℃, an upper hot press and a lower hot press are closed, and the pressure intensity range of the hot press is 10-100kgf/cm 2 Foaming time is 30-120min; opening a platen of the hot press to relieve pressure; transferring the mold onto a platen of a cold press, which is connected with a cooling device in advance to have enough cooling power, maintaining the temperature of the platen at 0-25 ℃, closing the upper and lower cold presses, and keeping the pressure of the press within 10-100kgf/cm 2 Cooling the die; and when the temperature of the mold is reduced to below 60 ℃, opening a platen of the cold press, removing the mold, and opening the mold to obtain the foam core material of the water sports board.
In the step 1), a rigid foam connecting plate is pre-buried at a lower die base of the foaming die for subsequent connection of flat bars; the rigid foam connecting plate is 0.04-0.05g/cm 3 Or 0.04-0.05g/cm 3 Polyurethane foam, or 0.04-0.05g/cm 3 Polyvinyl chloride foam.
The preferable specific method for the compression molding of the crude blank of the water sports board in the step 4) is as follows: placing the prepreg inclusion into a forming die of a moving plate, closing the die and effectively locking the die; transferring to a platen of a hot press, connecting the platen with a heating device in advance to have enough heating power, maintaining the temperature of the platen at 100-160 ℃, closing the upper and lower hot presses, and keeping the pressure of the press within 10-100kgf/cm 2 Forming for 50-120min, opening a platen of a hot press to discharge pressure; transferring the mold onto a platen of a cold press, which is connected with a cooling device in advance to have enough cooling power, maintaining the temperature of the platen at 0-25 ℃, closing the upper and lower cold presses, and keeping the pressure of the press within 10-100kgf/cm 2 And cooling the mould, opening a platen of the cold press when the temperature of the mould is reduced to below 60 ℃, removing the mould, unlocking the mould and opening the mould to obtain the light-weight rough blank of the water sports board.
And 3) when the prepreg inclusion is prepared, the fiber prepreg consists of two layers of glass fiber prepreg cloth close to the foaming core material and one layer of 3k carbon fiber prepreg cloth outside the glass fiber prepreg cloth.
The crude embryo of the water sports board obtained by the invention has excellent performance. When the fatigue test is carried out, after 30000 times of reciprocating motions are carried out at the middle position of the forefoot sleeve hole with the set force value of 50kg, the interface between the surface fiber composite material and the EEC foaming core material inside is kept intact;
when the lateral bending resistance test is carried out on the rough blank of the water sports board, the water sports board is fixed on a vertical testing device, a flat bar (9) with the length of 850mm is fixed on a base (8), a 50kg weight (10) is hung on the top of the outer end of the flat bar, downward acting force is loaded by utilizing the weight dead weight, the bending test is carried out on the water sports board in two directions of the base respectively, and a fiber layer at the base and an internal foaming core material are kept intact;
when the stretching resistance test is carried out on the rough blank of the water sports board, the two ends of the water sports board are pressed near the middle part, the water sports board is stretched upwards from the base groove of the water sports board by a universal pulling machine, the stretching speed is 25mm/min, the stretching is stopped when the stretching force reaches 500kg, and the fiber layer of the base structure and the foaming core material inside are kept intact.
Compared with the existing water sports board forming material and forming process, the novel light water sports board HEM (thermal expansion compression molding process Heat Expansion Molding) forming material and forming process disclosed by the invention have the following beneficial effects:
1. excellent seawater adsorption resistance. According to the invention, the organic silicon functional groups are modified by using tetramethyl cyclotetrasiloxane, allyl glycidyl ether and styrene, so that the hydrophobic liquid or colloidal organic silicon modified epoxy polymer SiEP is prepared, and the core material and the final water sports board have excellent seawater absorption resistance.
2. Excellent rebound performance. The modification of polyether functional groups is carried out by adopting amino-terminated polyether with proper molar ratio, so that the toughness of the core material is further improved, and the rebound resilience performance is excellent, so that the surfboard can rebound well to recover the appearance shape when being slightly collided and deformed in the use process, and the service life of the surfboard is prolonged.
3. High expansion performance and controllable foaming density. The EEC of the epoxy expansion core material of the invention adopts the synergistic effect of the foaming agent and the resin system to obtain the expansion core material with the expansion multiplying power range of 50-150 times and the expansion foaming core material density of 0.01-0.05 g/cm 3 Can obtain a concentration of less than 0.025g/cm 3 The expanded foam core material with the density, which is not available in the conventional foam materials on the market at present and is suitable for the foam materials which are molded at medium and low temperature, further leads to the unexpected light weight effect of the surfboard. The required EEC weight can be calculated according to the required density and the volume of the die cavity, the EEC sheet is weighed and placed in a foaming die, and finally the expansion foaming core material with the designed density is obtained through foaming molding, so that the density is controllable.
4. According to the invention, an epoxy thermosetting system is introduced into the EEC formula of the epoxy expansion core material, so that the foaming core material can realize ring-opening crosslinking reaction under the medium-low temperature condition, the crosslinking density of the resin system is improved, the produced surfboard is further prevented from swelling deformation under the baking condition of 80 ℃, the difficulty of heat absorption deformation of the carbon fiber surfboard under the high ultraviolet radiation at sea is overcome, in addition, the epoxy resin component in the EEC and the epoxy resin in the prepreg are of the same type, so that the interface of the epoxy resin component and the epoxy resin component has better bonding strength, and skin delamination of the surfboard in the use process is effectively prevented.
5. The product has full appearance and good strength. The invention adopts the synergistic effect of the foaming agent and the resin system, not only realizes the thermal expansion compression molding of the core material and achieves the effect of controllable expansion, but also can lead the fiber product to have a fuller appearance and better interlayer bonding force of the prepreg due to the expansion force from inside to outside of the foaming agent in the core material under the medium-low temperature condition in the thermal molding stage of the product, thereby improving the strength performance of the product.
6. The loss is reduced, and the cost is lowered. The EEC material can meet the requirements of HEM thermal expansion compression molding process, foam in a mold, and is different from the CNC addition process of the traditional foam, so that the processing loss and waste of the material are avoided, and the cost is reduced.
7. The HEM forming process is different from the traditional hand lay-up process, and realizes compression molding in the field of water sport boards, so that the weight and quality controllability of products are improved, the appearance size precision is improved, the production efficiency is greatly improved, and the production environment is greatly improved.
Drawings
FIG. 1 shows a device for testing foaming ratio of the present invention
Figure 2 is a schematic cross-sectional view of a surfboard blank of the present invention
FIG. 3 shows a lateral bending resistance test device according to the present invention
Detailed Description
The technical scheme of the present invention is further described in detail below by examples, which are only preferred embodiments for illustrating the technical scheme of the present invention, and are not to be construed as limiting the present invention.
In the present invention, "parts" refer to parts by weight. The steps of the specific embodiment are shown in the table one.
List one
Example 1
The novel light water sports board HEM (thermal expansion compression molding process Heat Expansion Molding) molding material is prepared by the following steps.
Step 1, firstly preparing an organosilicon modified epoxy polymer: the hydrophobic organosilicon modified epoxy polymer, siEP for short, is prepared from tetramethyl cyclotetrasiloxane, allyl glycidyl ether and styrene.
Tetramethyl cyclotetrasiloxane (CAS: 2370-88-9, D4H for short), allyl glycidyl ether (CAS: 106-92-3, AGE for short), styrene (CAS: 100-42-5, ST for short), and the molar ratio of the three is 1:2:2; the method comprises the following specific steps: the whole process is carried out in an inert gas-protected reaction kettle, a certain amount of D4H is added, the temperature is maintained at 80 ℃, 25% of AGE and 25% of ST mixture are added under the stirring of 500rpm, 20-60ppm of platinum catalyst (CAS: 68478-92-2) is added dropwise, the stirring of 500rpm is maintained for 10min, the rest 75% of AGE and 75% of ST mixture are added dropwise, the dropping speed of the process is controlled to maintain the temperature range of 80-90 ℃, after the dropping is completed, the stirring reaction is maintained for 4 hours, then the temperature is increased to 120 ℃, the low-boiling-point solvent is removed under the reduced pressure, the absolute pressure is 10-20KPa, and the transparent liquid organosilicon modified epoxy polymer SiEP is obtained after discharging.
The resulting SiEP includes two isomers of the following structural formula:
step 2, preparing an organosilicon polyether modified epoxy polymer, siEEP for short
The components and proportions corresponding to example 1 in Table II are as follows:
1. the epoxy resin EP adopts E-44 parts, E-44 is the general product model in the field, the qualified products of various manufacturer models can be selected,
2. 8 parts by weight of the organosilicon modified epoxy polymer SiEP obtained in the step 1, 10 parts of 1, 6-hexanediol diglycidyl ether as 3 and an epoxy reactive diluent ED are adopted, the organosilicon modified epoxy polymer SiEP is a general product model in the field, the qualified products of various manufacturer models can be obtained,
4. the number of moles of N-H bonds contained in the charged amount of the amine-terminated polyether PEA is 0.3 times of the number of moles of epoxy groups in the system, the product D400 which is a common product in the field is selected, the qualified products of all manufacturer types can be selected,
the preparation process is as follows:
and (2) weighing the epoxy resin E-44 according to the proportion, adding the organosilicon modified epoxy polymer SiEP obtained in the step (1) and the 1, 6-hexanediol diglycidyl ether into a reaction kettle, maintaining the temperature at 70 ℃, stirring and mixing at 300-900rpm for 2-4h, adding PEA according to the calculated amount of the materials, stirring and mixing at 300-900rpm for 1-2h, sealing at room temperature and standing for more than 12h for later use, and obtaining the organosilicon polyether modified epoxy polymer SiEEP, which is named as SiEEP-1# in a second table.
Watch II
In fact, in the present invention, the epoxy resin EP may be one or any two or more of the epoxy resins E-06, E-12, E-20, E-44 and E-51 in addition to the components described in the present embodiment 1; the active epoxy diluent ED can be one or any two or more of benzyl glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, diglycidyl ether, 1, 6-hexanediol diglycidyl ether and polypropylene glycol diglycidyl ether; the amino-terminated polyether can be one or any combination of two or more of polyoxypropylene diamine D230, polyoxypropylene diamine D400, polyoxyethylene diamine ED600 and polyoxyethylene diamine ED 900.
Step 3, preparing an organosilicon polyether modified epoxy emulsion, namely AQ-SiEEP
Watch III
Adding a solvent into the organosilicon polyether modified epoxy polymer SiEEP obtained in the step 2 for emulsification and dilution to obtain an organosilicon polyether modified epoxy emulsion, namely AQ-SiEEP;
the emulsified formulation in the invention: 100 parts by weight of organosilicon polyether modified epoxy polymer SiEEP obtained in the step 2, 10-20 parts by weight of cosolvent and 60-100 parts by weight of main solvent. The cosolvent is one or any combination of more than two of isopropanol, ethylene glycol butyl ether, ethylene glycol, propylene glycol methyl ether and dipropylene glycol butyl ether. The main solvent may be water or other solvents.
In the present example 1, the proportions of example 1 shown in Table III,
weighing the organosilicon polyether modified epoxy polymer SiEEP-1# obtained in the step 2 and cosolvent isopropanol, sequentially adding into an emulsifying device, heating to 80 ℃, stirring at 900-1000rpm uniformly for 0.5 hours, cooling to 60 ℃, stirring at 3000rpm, and dripping a main solvent H with a preset amount in 1.5 hours 2 O, maintaining high-rotation-speed shearing emulsification for 1 hour, and then cooling to 40 ℃, and maintaining high-rotation-speed 3000rpm stirring for 1 hour to obtain the organosilicon polyether modified epoxy emulsion AQ-SiEEP. In this example, the main solvent is preferably water, and the resulting emulsion is a silicone polyether modified epoxy emulsion AQ-SiEEP, designated AQ-SiEEP-1# in Table three. The main solvent in this example 1 is preferably water, and one or a combination of two or more of isopropyl alcohol, ethylene glycol butyl ether, ethylene glycol, propylene glycol methyl ether, and dipropylene glycol butyl ether may be used as the main solvent.
Step 4, preparing coating foaming material
The components and the proportions shown in the example 1 of the fourth table are taken, the organosilicon polyether modified epoxy emulsifier AQ-SiEEP, water, dicyandiamide DICY, an accelerator and a foaming agent are sequentially measured and added into a stirring kettle according to the proportion, the stirring speed is 1000-1200rpm, the stirring is carried out for about 1 hour, and the coating foaming material is obtained and recorded as EEC-1# in the fourth table for use in the step 5.
The silicone polyether modified epoxy emulsion AQ-SiEEP in this example is the aqueous silicone polyether modified epoxy emulsion AQ-SiEEP-1# obtained in step 3 of this example 1.
The accelerator in this step is an organic urea accelerator, and 1,1' - (4-methyl-m-phenylene) bis (3, 3-dimethylurea) CAS is 17526-94-2.
The foaming agent is a thermal expansion microsphere foaming agent which is selected from 551DU40, 461DU20, 051DU40, 920DU20 and 920DU40 of NOURYON; or F-48D, F-50D, F-65D, MSH-340, MSH-550, F-100MD, F-78KD, F-82D of MATSUMOTO; or SEKISUI EHM204, EHM302, EM303, EM406, EML 101.
Table four
Step 5, preparing an epoxy expansion core material (Epoxy Expand Core is EEC for short)
Coating the coating foaming material EEC-1# obtained in the step 4 on release paper through a coating device in the prior art, and then obtaining the epoxy expansion core material EEC which can be peeled from the release paper through a drying process, wherein the EEC-1# is marked as EEC-1# in a table IV.
In example 1, comma knife coating is preferable, and either reverse roll coating or extrusion coating may be used. The square gram weight range of the release paper is selected to be 100-150g/m 2 The peeling force of the coating surface can be 0.4-0.6N/25 mm.
The dried EEC-1# was weighed to give a square gram weight of 120g/m 2 。
In order to test the foaming ratio of EEC-1#, the self-made foaming ratio testing device T002 is shown in figure 1, and is a cubic mold, wherein the middle part of the cubic mold is a mold groove with the length of 6cm multiplied by 6cm, the hollow part corresponds to a pressing block with the length of 5.8cm multiplied by 3cm which can be pushed in and taken out, and the top of the pressing block is provided with a handle. The testing method comprises the following steps:
1. pre-heating a T002 die and a pressing block on a pneumatic hot press at 150 ℃ for 25min;
2. cutting EEC-1#, sampling a square sheet with the volume of 60mm multiplied by 60mm, calculating the volume of the square sheet to be the volume before foaming, putting the square sheet into a test die, covering a pressing block, and providing test pressure of 1atm by the dead weight of the pressing block;
3. foaming temperature is 150+/-5 ℃ for 20min, and taking out the foam;
4. measuring the size of the foam body by using a vernier caliper;
5. expansion ratio = volume after foaming/volume before foaming. The foaming ratio obtained in this example 1 was 135 times, and the results are shown in Table IV.
And 6, obtaining an epoxy expansion core material EEC-1# by utilizing the step 5, and forming the lightweight water sports board by adopting a thermal expansion compression molding process Heat Expansion Molding (HEM for short).
In this example, a surfboard (the rest of the sports boards may be used) was selected as a molded product, and molded according to the data corresponding to example 1 in table five.
TABLE five
The specific forming process is as follows:
STEP1, mold preparation and foam core HEM molding:
the foaming mold is manufactured according to the design size of the surfboard. The inner cavities of the upper and lower dies are cleaned, a release agent is coated, and a rigid foam connecting plate is pre-buried at the base of the bottom die, as shown in figure 2, the rigid foam connecting plate 3 is used for connecting flat bars at the injection molding hydrofoil groove 5 later, and the material of the rigid foam connecting plate 3 is preferably 0.04-0.05g/cm 3 Is a polyimide foam of (a). The outer surface of the rigid foam connecting plate 3 is provided with a glue coating layer 4. According to the size of the foaming mould, the volume of the foaming cavity is multiplied by the density of the designed core material to be 0.015g/cm 3 Calculating the weight of EEC of the injected epoxy expansion core material; weighing epoxy of corresponding weightPlacing an expansion core material EEC-1# into the foaming mold, closing the mold and effectively locking the mold;
the foaming mould is transferred to a platen of a hot press, the platen of the hot press is connected with a heating device in advance, the temperature of the platen is maintained at about 140 ℃ with enough heating power, an upper hot press and a lower hot press are closed, and the pressure range of the hot press is 50kgf/cm 2 About, the foaming time is about 120 min; opening a platen of the hot press to relieve pressure; transferring the mold onto a platen of a cold press, which is connected with a cooling device in advance to have enough cooling power, maintaining the temperature of the platen at 0-25 ℃, closing the upper and lower cold presses, and keeping the pressure range of the press at 50kgf/cm 2 Cooling the die; when the temperature of the mold was lowered below 60 ℃, the platen of the cold press was opened, the mold was removed, and the mold was opened, to obtain a surfboard foam core 6 of example 1, as shown in the schematic diagram of fig. 2.
STEP2, preparation of prepreg inclusion
The foam core material 6 obtained in STEP1 is lightly polished on the surface by using 150# sand paper, so as to eliminate trace release agents possibly attached to the surface of the core material, then an air gun is used for blowing and cleaning, a plurality of layers of fiber prepreg are wrapped on the surface of the foam core material according to the existing layering structure, and a prepreg inclusion is obtained, and the structure schematic diagram is shown in figure 2. The fiber prepreg consists of two layers of glass fiber prepregs 2 close to the foaming core material and one layer of 3k carbon fiber prepreg 1 outside the two layers of glass fiber prepregs, and can also be of other layered structures, and the fiber prepreg is set according to actual demands of products.
STEP3 and surfboard rough blank compression molding
Placing the prepreg inclusion into a forming die of a surfboard, closing the die and effectively locking the die; transferring to a platen of a hot press, wherein the platen of the hot press is connected with a heating device in advance, the temperature of the platen is maintained at about 140 ℃ with enough heating power, the upper and lower hot presses are closed, and the pressure intensity of the press is 50kgf/cm 2 About, the pressure is 10-10050kgf/cm 2 The molding time is 90min, and the platen of the hot press is opened to discharge pressure; transferring the mold onto a platen of a cold press, which is connected with a cooling device in advance and has enough cooling power, maintaining the temperature of the platen at 0-25 ℃, and closing the upper and lower coolingA press having a pressure range of 50kgf/cm 2 Cooling the mould, opening the platen of the cold press when the temperature of the mould is reduced to below 60 ℃, removing the mould, unlocking the mould and opening the mould to obtain a lightweight surfboard rough blank, namely SURF-2#.
And 7, performing fatigue test, lateral bending resistance test and tensile test on the obtained rough blank of the surfboard, wherein the fatigue test, the lateral bending resistance test and the tensile test are shown in a sixth table.
1. Fatigue test
The surfing board is locked and fixed on a fatigue testing machine, the fatigue testing machine is provided with two parallel air cylinders, one air cylinder is used for fixing the surfing board, and the other air cylinder makes 30000 reciprocating motions at the middle position of a front foot sleeve hole with a set force value of 50 kg.
Qualified test results: the fiber composite material on the surface and the EEC foam core material inside the surface have no cracking and delamination at the interface after 30000 times of fatigue test.
2. Lateral bending resistance test
As shown in fig. 3, the bending resistance test device is that the surfing board 7 is fixed on a vertical test device, and the 850mm long integrated flat bar 9 is fixed on the base 8 of the surfing board, and the width of the base is 90mm. A 50kg weight 10 was hung on top of the flat bar. Utilize the weight dead weight to produce decurrent effort, test base's structural strength. The two directions of the surfboard base are respectively loaded with bending and tested once.
Qualified test results: the structure of the base is not broken by the fiber layer and the inner foam core material.
3. Tensile test
The related tool comprises: can load 500kg of universal tensile machine and fixing clamp.
Pressing and fixing the near middle parts of two ends of the surfing board on a test machine by using a pressing rod, wherein the pressing rod at the front end is required to be 25cm away from the hydrofoil groove; the T-shaped screw cap is centrally placed in a base groove of the surfing board and locked and fixed; the machine can be upwards stretched by a universal tensile machine capable of loading 500kg, the stretching speed is 25mm/min, and the machine stops when the stretching force reaches 500kg, or the machine stops in advance when the machine breaks midway.
Qualified test results: the base structure does not exhibit delamination fracture of the fibrous layer from the inner foam core.
4. Water absorption test
And (3) in the testing process, cutting the fiber skin by a blade to a length of 3cm and a depth of 1cm at the right middle position of the bottom of the surfboard, and penetrating the fiber skin into the EEC foaming core material. The surfboard floats on the surface of seawater, the damaged port is completely contacted with the seawater, and the tested environment temperature is 25 ℃ and the relative humidity is 40% -50%.
The weight/g of the surfboard before testing is recorded as M 0 After 12 hours of testing, the surfboard was removed and the surface was wiped with seawater until no visible water droplets were present, and the weight/g was recorded by weighing and recorded as M a The method comprises the steps of carrying out a first treatment on the surface of the Calculate the relative water absorption = M a -M 0 =30g, noted in table six. Qualified test results: the relative water absorption is less than 100g.
TABLE six
Example 2
Step 1, firstly preparing the organosilicon modified epoxy polymer.
The components, proportions and preparation method are the same as in example 1.
Step 2, preparing the organosilicon polyether modified epoxy polymer
The preparation process was the same as in example 1 except that the components were selected and compounded as shown in example 2 of Table II, and the resulting silicone polyether modified epoxy polymer, noted SiEEP-2# in Table II.
Step 3, preparing the organosilicon polyether modified epoxy emulsion
The preparation method was the same as in example 1 except that the selection and proportions of the components were as shown in example 2 of Table three, and the resulting silicone polyether modified epoxy emulsion, designated AQ-SiEEP-2# in Table three.
Step 4, preparing a coating material
The preparation was carried out as in example 1, except that the components were selected and proportioned as in example 2 of Table four, and the resulting coating was corresponding to EEC-2# in Table four.
Step 5, preparing the epoxy expansion core material
The preparation method is the same as in example 1, and the EEC-2# square gram weight of the epoxy expansion core material obtained after coating and drying is 240g/m 2 Record in Table IV.
The expansion ratio of EEC-2# was 115 times as measured by the expansion ratio test method of example 1, and is also shown in Table IV.
Step 6, using step 5 to obtain EEC-2# of epoxy expansion core material, forming the surfing board by adopting a thermal expansion compression molding process HEM, wherein the specific process is the same as the step six of the embodiment, except that each parameter and each component are shown in the embodiment 2 in the table five. The resulting surfboard blank was designated SURF-5#.
Step 7, performing fatigue test, lateral bending resistance test and tensile test on the obtained surfboard rough SURF-5# according to the method and equipment in step 7 of the embodiment 1, wherein the results are shown in the corresponding description of the sixth embodiment 2.
Example 3
Step 1, firstly preparing the organosilicon modified epoxy polymer.
The components, proportions and preparation method are the same as in example 1.
Step 2, preparing the organosilicon polyether modified epoxy polymer
The preparation process was the same as in example 1 except that the components were selected and compounded as shown in example 3 of Table II, and the resulting silicone polyether modified epoxy polymer, noted SiEEP-3# in Table II.
Step 3, preparing the organosilicon polyether modified epoxy emulsion
The preparation method was the same as in example 1 except that the selection and proportions of the components were as shown in example 3 of Table three, and the resulting silicone polyether modified epoxy emulsion, designated AQ-SiEEP-3# in Table three.
Step 4, preparing a coating material
The preparation was carried out as in example 1, except that the components were selected and proportioned as shown in example 3 of Table four, and the resulting coating was corresponding to EEC-3# in Table four.
Step 5, preparing the epoxy expansion core material
The preparation method is the same as in example 1, and the EEC-3# square gram weight of the epoxy expansion core material obtained after coating and drying is 289g/m 2 Record in Table IV.
The expansion ratio of EEC-3# was 50 times as measured by the expansion ratio test method of example 1, and is also shown in Table IV.
Step 6, using step 5 to obtain EEC-3# of epoxy expansion core material, forming surfing board by thermal expansion compression molding process HEM, wherein the specific process is the same as step six of the embodiment, except that each parameter and component are shown in the embodiment 3 in the table five. The resulting surfboard blank was designated SURF-1#.
Step 7, performing fatigue test, lateral bending resistance test and tensile test on the obtained surfboard rough SURF-1# according to the method and equipment in the step 7 of the embodiment 1, wherein the results are shown in the corresponding description of the sixth embodiment 3.
Example 4
Step 1, firstly preparing the organosilicon modified epoxy polymer.
The components, proportions and preparation method are the same as in example 1.
Step 2, preparing the organosilicon polyether modified epoxy polymer
The preparation method is the same as in example 1 except that the components are selected and proportioned according to the formula shown in example 4 (i.e., example 2) in Table II, and the obtained silicone polyether modified epoxy polymer is SiEEP-2# in Table II.
Step 3, preparing the organosilicon polyether modified epoxy emulsion
The preparation method is the same as in example 1 except that the components are selected and proportioned according to the composition shown in example 4 in Table three, and the obtained organosilicon polyether modified epoxy emulsion is AQ-SiEEP-2# in Table three.
Step 4, preparing a coating material
The preparation was carried out as in example 1, except that the components were selected and proportioned as shown in example 4 of Table four, and the resulting coating was corresponding to EEC-4# in Table four.
Step 5, preparing the epoxy expansion core material
The preparation method is the same as in example 1, and the EEC-4# square gram weight of the epoxy expansion core material obtained after coating and drying is 100g/m 2 Record in Table IV.
The expansion ratio of EEC-4# was 130 times as measured by the expansion ratio test method of example 1, and is also shown in Table IV.
Step 6, using step 5 to obtain EEC-4# of epoxy expansion core material, forming the surfing board by adopting a thermal expansion compression molding process HEM, wherein the specific process is the same as the step 6 of the embodiment, except that each parameter and each component are shown in the embodiment 4 in the table five. The resulting surfboard blank was designated SURF-6#.
Step 7, performing fatigue test, lateral bending resistance test and tensile test on the obtained surfboard rough SURF-6# according to the method and equipment in step 7 of the embodiment 1, wherein the results are shown in the corresponding description of the sixth embodiment 4.
Example 5
Step 1, firstly preparing the organosilicon modified epoxy polymer.
The components, proportions and preparation method are the same as in example 1.
Step 2, preparing the organosilicon polyether modified epoxy polymer
The preparation method is the same as in example 1 except that the components are selected and proportioned according to the method shown in example 5 (i.e. example 3) in Table II, and the obtained silicone polyether modified epoxy polymer is SiEEP-3#, in Table II.
Step 3, preparing the organosilicon polyether modified epoxy emulsion
The preparation method is the same as in example 1 except that the components are selected and proportioned according to the method shown in example 5 (i.e. example 3) in Table three, and the obtained silicone polyether modified epoxy emulsion is AQ-SiEEP-3# in Table three.
Step 4, preparing a coating material
The preparation was carried out as in example 1, except that the components were selected and proportioned as shown in example 5 of Table IV, and the resulting coating was corresponding to EEC-5# in Table IV.
Step 5, preparing the epoxy expansion core material
The preparation method is the same as in example 1, and the EEC-5# square gram weight of the epoxy expansion core material obtained after coating and drying is 300g/m 2 Record in Table IV.
The foaming ratio of EEC-5# was 85-fold as measured by the foaming ratio test method of example 1, and is also reported in Table IV.
This example 5 does not proceed with steps 6 and 7. The preparation steps and effects are the same as those of other examples, and are not repeated.
Example 6
Step 1, firstly preparing the organosilicon modified epoxy polymer.
The components, proportions and preparation method are the same as in example 1.
Step 2, preparing the organosilicon polyether modified epoxy polymer
The preparation method is the same as in example 1 except that the components are selected and proportioned according to example 6 in Table II, and the obtained silicone polyether modified epoxy polymer is SiEEP-4# in Table II.
Step 3, preparing the organosilicon polyether modified epoxy emulsion
The preparation method is the same as in example 1 except that the components are selected and proportioned according to the method shown in example 6 (i.e. example 7) in Table III, and the obtained silicone polyether modified epoxy emulsion is AQ-SiEEP-4# in Table III.
Step 4, preparing a coating material
The preparation was carried out as in example 1, except that the components were selected and proportioned as shown in example 6 of Table IV, and the resulting coating was corresponding to EEC-6# in Table IV.
Step 5, preparing the epoxy expansion core material
The preparation method is the same as in example 1, and the EEC-6# square gram weight of the epoxy expansion core material obtained after coating and drying is 240g/m 2 Record in Table IV.
The expansion ratio of EEC-5# was 62 times as measured by the expansion ratio test method of example 1, and is also shown in Table IV.
This example 6 does not proceed with steps 6 and 7. The preparation steps and effects are the same as those of other examples, and are not repeated.
Example 7
Step 1-3 is step 1-3 of example 6.
Step 4, preparing a coating material
The preparation was carried out as in example 1, except that the components were selected and proportioned as shown in example 7 of Table IV, and the resulting coating was corresponding to EEC-7# in Table IV.
Step 5, preparing the epoxy expansion core material
The preparation method is the same as in example 6, and the EEC-7# square gram weight of the epoxy expansion core material obtained after coating and drying is 120g/m 2 Record in Table IV.
The foaming ratio of EEC-5# was 60 times as measured by the foaming ratio test method of example 1, and is also shown in Table IV.
This example 7 does not proceed with steps 6 and 7. The preparation steps and effects are the same as those of other examples, and are not repeated.
Example 8
Step 1, firstly preparing the organosilicon modified epoxy polymer.
The components, proportions and preparation method are the same as in example 1.
Step 2, preparing the organosilicon polyether modified epoxy polymer
The preparation method is the same as in example 1 except that the components are selected and proportioned according to the formula shown in example 8 (i.e., example 2) in Table II, and the obtained silicone polyether modified epoxy polymer is SiEEP-2# in Table II.
Step 3, preparing the organosilicon polyether modified epoxy emulsion
The preparation method is the same as in example 1 except that the components are selected and proportioned according to the method shown in example 8 (i.e. example 2) in Table III, and the obtained silicone polyether modified epoxy emulsion is AQ-SiEEP-2# in Table III.
Step 4, preparing a coating material
The preparation was carried out as in example 1, except that the components were selected and proportioned as shown in example 8 of Table four, and the resulting coating was corresponding to EEC-8# in Table four.
Step 5, preparing the epoxy expansion core material
The preparation method is the same as in example 1, and the EEC-4# square gram weight of the epoxy expansion core material obtained after coating and drying is 100g/m 2 Record in Table IV.
The expansion ratio of EEC-4# was 120 times as measured by the expansion ratio test method of example 1, and is also shown in Table IV.
Step 6, using step 5 to obtain EEC-8# of epoxy expansion core material, forming the surfing board by adopting a thermal expansion compression molding process HEM, wherein the specific process is the same as the step 6 of the embodiment, except that each parameter and each component are shown in the embodiment 8 in the table five. The resulting surfboard blank was designated SURF-4#.
Step 7, performing fatigue test, lateral bending resistance test and tensile test on the obtained surfboard rough SURF-6# according to the method and equipment in the step 7 of the embodiment 1, wherein the results are shown in the corresponding description of the sixth embodiment 8.
Example 9
Step 1, firstly preparing the organosilicon modified epoxy polymer.
The components, proportions and preparation method are the same as in example 1.
Step 2, preparing the organosilicon polyether modified epoxy polymer
The preparation method is the same as in example 1 except that the components are selected and proportioned according to the method shown in example 9 (i.e. example 1) in Table II, and the obtained silicone polyether modified epoxy polymer is SiEEP-1# in Table II.
Step 3, preparing the organosilicon polyether modified epoxy emulsion
The preparation method is the same as in example 1 except that the components are selected and proportioned according to the method shown in example 9 (i.e. example 1) in Table III, and the obtained silicone polyether modified epoxy emulsion is AQ-SiEEP-1# in Table III.
Step 4, preparing a coating material
The preparation was carried out as in example 1, except that the components were selected and proportioned as shown in example 9 of Table four, and the resulting coating was corresponding to EEC-9# in Table four.
Step 5, preparing the epoxy expansion core material
The preparation method is the same as in example 1, and the EEC-9# square gram weight of the epoxy expansion core material obtained after coating and drying is 240g/m 2 Record in Table IV.
The expansion ratio of EEC-4# was 140 times as measured by the expansion ratio test method of example 1, and is also reported in Table IV.
Step 6, using step 5 to obtain EEC-9# of epoxy expansion core material, forming the surfboard by adopting thermal expansion compression molding process HEM, wherein the specific process is the same as the step 6 of the embodiment, except that each parameter and each component are shown in the embodiment 9 in the table five. The resulting surfboard blank was designated SURF-3#.
Step 7, performing fatigue test, lateral bending resistance test and tensile test on the obtained surfboard rough SURF-3# according to the method and equipment in the step 7 of the embodiment 1, wherein the results are shown in the corresponding description of the sixth embodiment 9.
Example 10
Step 1, firstly preparing the organosilicon modified epoxy polymer.
The components, proportions and preparation method are the same as in example 1.
Step 2, preparing the organosilicon polyether modified epoxy polymer
The preparation method is the same as in example 1 except that the components are selected and proportioned according to example 10 in Table II, and the obtained silicone polyether modified epoxy polymer is SiEEP-5# in Table II.
Step 3, preparing the organosilicon polyether modified epoxy emulsion
The preparation method is the same as in example 1 except that the components are selected and proportioned according to example 10 in Table three, and the obtained organosilicon polyether modified epoxy emulsion is AQ-SiEEP-5# in Table three.
Step 4, preparing a coating material
The preparation was carried out as in example 1, except that the components were selected and proportioned as shown in example 10 of Table IV, and the resulting coating was corresponding to EEC-10# in Table IV.
Step 5, preparing the epoxy expansion core material
The preparation method is the same asExample 1 epoxy expanded core material EEC-10# square gram weight obtained after coating and drying was 225g/m 2 Record in Table IV.
The expansion ratio of EEC-4# was 65 times as measured by the expansion ratio test method of example 1, and is also shown in Table IV.
This example 10 does not proceed to steps 6 and 7. The preparation steps and effects are the same as those of other examples, and are not repeated.
Claims (17)
1. The novel light water sports board HEM molding material is characterized by being prepared through the following steps:
step 1, preparing an organosilicon modified epoxy polymer: preparing a hydrophobic organosilicon modified epoxy polymer, siEP for short, by using tetramethyl cyclotetrasiloxane, allyl glycidyl ether and styrene;
step 2, preparing an organosilicon polyether modified epoxy polymer, siEEP for short, by using the following components in proportion:
1) 50-80 parts by weight of epoxy resin, EP for short,
2) The organosilicon modified epoxy polymer SiEP obtained in the step 1 is 5-10 parts by weight,
3) Epoxy reactive diluent, ED for short, 5-10 weight portions,
4) The mole number of N-H bonds contained in the amino-terminated polyether, PEA for short, is 0.2-0.5 times of the mole number of epoxy groups in the system;
step 3, adding the organosilicon polyether modified epoxy polymer SiEEP obtained in the step 2 into a solvent, emulsifying and diluting to obtain an organosilicon polyether modified epoxy emulsion, namely AQ-SiEEP; the formula adopted is as follows: the organosilicon polyether modified epoxy polymer SiEEP obtained in the step 2 is 100 weight parts, the cosolvent is 10-20 weight parts, and the main solvent is 60-100 weight parts;
step 4, preparing a coating foaming material: the composite material is prepared by mixing the following components in proportion:
1) 50-70 parts by weight of organosilicon polyether modified epoxy emulsifier AQ-SiEEP,
2) 0 to 30 parts by weight of water,
3) The dicyandiamide DICY dosage is multiplied by the active hydrogen equivalent according to 0.9 to 1.0 times of the epoxy mole number of the organosilicon polyether modified epoxy emulsion AQ-SiEEP,
4) The usage amount of the accelerator is 0.5-1.5 times of the dicyandiamide DICY feeding weight,
5) 50-100 parts by weight of foaming agent;
step 5, preparing an epoxy expansion core material, namely EEC: coating the coating foaming material obtained in the step 4 on release paper, and drying to obtain an epoxy expansion core material EEC which can be peeled from the release paper, wherein the foaming multiplying power range of the epoxy expansion core material EEC is 50-150 times, and the density range of the foaming core material obtained after thermal expansion is 0.01-0.05g/cm 3 。
2. The novel lightweight water sports board HEM molding material of claim 1, wherein in the step 1, the molar ratio of tetramethyl cyclotetrasiloxane, allyl glycidyl ether and styrene is 1:2:2;
the preparation process comprises the following steps: adding tetramethyl cyclotetrasiloxane into a reaction kettle protected by inert gas, maintaining the temperature at 80 ℃, adding a mixture of 25% allyl glycidyl ether and 25% styrene under stirring at 500rpm, dropwise adding 20-60ppm of platinum catalyst with CAS number of 68478-92-2, maintaining stirring at 500rpm for 10min, dropwise adding the rest mixture of 75% allyl glycidyl ether AGE and 75% styrene ST, maintaining the temperature range of a dripping acceleration maintaining system in the process at 80-90 ℃, maintaining stirring for 4 hours after the dripping is completed, then heating to 120 ℃, removing the low-boiling point solvent under reduced pressure, and obtaining transparent liquid by discharging, wherein the absolute pressure is 10-20 KPa.
3. The novel lightweight water sports board HEM molding material of claim 2, wherein the SiEP of step 1 comprises two isomers of the following structural formula:
4. the novel lightweight water sports board HEM molding material of claim 1, wherein in said step 2, said epoxy resin is one or a combination of any two or more of epoxy resin E-06, epoxy resin E-12, epoxy resin E-20, epoxy resin E-44 and epoxy resin E-51;
The epoxy reactive diluent is one or any two or more of benzyl glycidyl ether, butyl glycidyl ether, phenyl glycidyl ether, diglycidyl ether, 1, 6-hexanediol diglycidyl ether and polypropylene glycol diglycidyl ether;
the amino-terminated polyether is one or a combination of any two or more of polyoxypropylene diamine D230, polyoxypropylene diamine D400, polyoxyethylene diamine ED600 and polyoxyethylene diamine ED 900.
5. The novel lightweight water sports board HEM molding material of claim 1, wherein the process of preparation in step 2: and (2) weighing epoxy resin EP according to a proportion, adding the organosilicon modified epoxy polymer SiEP obtained in the step (1) and an epoxy reactive diluent ED into a reaction kettle, maintaining the temperature at 70 ℃, stirring and mixing for 2-4 hours at 300-900rpm, adding amino-terminated polyether PEA according to the calculated amount of the materials, stirring and mixing for 1-2 hours at 300-900rpm, sealing at room temperature, and standing for more than 12 hours for standby, thereby obtaining the organosilicon polyether modified epoxy polymer SiEEP.
6. The novel lightweight water sports board HEM molding material of claim 1, wherein the primary solvent in step 3 is water; the cosolvent is one or any two or more than two of isopropanol, ethylene glycol butyl ether, ethylene glycol, propylene glycol methyl ether and dipropylene glycol butyl ether.
7. The novel lightweight water sports board HEM molding material of claim 6, wherein the specific practice of step 3 is: and (2) weighing the organosilicon polyether modified epoxy polymer SiEEP and the cosolvent obtained in the step (2) according to the proportion, sequentially adding the organosilicon polyether modified epoxy polymer SiEEP and the cosolvent into an emulsifying device, heating to 80 ℃, uniformly stirring at 900-1000rpm for 0.5 hours, cooling to 60 ℃, dropwise adding the main solvent while stirring at 3000rpm within 1.5 hours, maintaining high-speed shearing and emulsifying for 1 hour, cooling to 40 ℃, and stirring at 3000rpm for 1 hour to obtain the organosilicon polyether modified epoxy emulsion AQ-SiEEP.
8. The novel lightweight water sports board HEM molding material of claim 1, wherein in said step 4, said accelerator is an organic urea accelerator, and 1,1' - (4-methyl-m-phenylene) bis (3, 3-dimethylurea) has a CAS of 17526-94-2.
9. The novel lightweight water sports board HEM molding material of claim 1, wherein in said step 4, said foaming agent is a thermally expansive microsphere;
the foaming agent is selected from 551DU40, 461DU20, 051DU40, 920DU20, 920DU40 of NOURYON;
or F-48D, F-50D, F-65D, MSH-340, MSH-550, F-100MD, F-78KD, F-82D of MATSUMOTO;
Or SEKISUI EHM204, EHM302, EM303, EM406, EML 101.
10. The novel lightweight water sports board HEM molding material of claim 1, wherein the epoxy expanded core material EEC coating obtained in step 5 has a square gram weight of 100-300g/m 2 。
11. A molding process for manufacturing a novel lightweight water sports board HEM by using the lightweight water sports board HEM molding material according to any of claims 1 to 10, comprising the steps of:
1) The volume of the foaming cavity is multiplied by the expected density of the core material to be 0.01-0.05g/cm according to the size of the foaming mould manufactured by the design size of the water sports board 3 Calculating the weight of EEC of the epoxy expansion core materialThe method comprises the steps of carrying out a first treatment on the surface of the Weighing an epoxy expansion core material EEC with corresponding weight, putting the EEC into the foaming mold, closing the mold and effectively locking the mold;
2) Transferring the foaming mould to a platen of a hot press to perform hot-press foaming expansion, and then performing cold pressing and cooling to obtain a foaming core material of the water sports board;
3) Wrapping fiber prepreg outside the foam core material of the water sports board to obtain a prepreg inclusion;
4) And (3) placing the prepreg inclusion into a forming die of the motion plate, hot-pressing on a platen of a hot press, and then cold-pressing and cooling to obtain the crude blank of the water motion plate.
12. The novel lightweight water sports board HEM molding process of claim 11, wherein the water sports board blank has a water absorption of 20g to 80g.
13. The novel lightweight water sports board HEM molding process of claim 11, wherein in step 2) the foaming mold is transferred to a platen of a hot press, the platen of the hot press is previously connected with a heating device to maintain the platen temperature at 120-160 ℃, the upper and lower hot presses are closed, and the pressure of the hot press ranges from 10 kgf/cm to 100kgf/cm 2 Foaming time is 30-120min; opening a platen of the hot press to relieve pressure; transferring the mold onto a platen of a cold press, which is connected with a cooling device in advance to have enough cooling power, maintaining the temperature of the platen at 0-25 ℃, closing the upper and lower cold presses, and keeping the pressure of the press within 10-100kgf/cm 2 Cooling the die; and when the temperature of the mold is reduced to below 60 ℃, opening a platen of the cold press, removing the mold, and opening the mold to obtain the foam core material of the water sports board.
14. The novel lightweight water sports board HEM molding process of claim 11, wherein in said step 1), said foaming mold, pre-burying a rigid foam connection board at the base of the lower mold for subsequent connection of flat bars; the rigid foam connecting plate is 0.04-0.05g/cm 3 Or 0.04-0.05g/cm 3 Polyurethane foam, or 0.04-0.05g/cm 3 Polyvinyl chloride foam.
15. The novel lightweight water sports board HEM molding process according to claim 11, wherein the specific practice of the step 4) molding the rough blank of the water sports board is as follows: placing the prepreg inclusion into a forming die of a moving plate, closing the die and effectively locking the die; transferring to a platen of a hot press, connecting the platen with a heating device in advance to have enough heating power, maintaining the temperature of the platen at 100-160 ℃, closing the upper and lower hot presses, and keeping the pressure of the press within 10-100kgf/cm 2 Forming for 50-120min, opening a platen of a hot press to discharge pressure; transferring the mold onto a platen of a cold press, which is connected with a cooling device in advance to have enough cooling power, maintaining the temperature of the platen at 0-25 ℃, closing the upper and lower cold presses, and keeping the pressure of the press within 10-100kgf/cm 2 And cooling the mould, opening a platen of the cold press when the temperature of the mould is reduced to below 60 ℃, removing the mould, unlocking the mould and opening the mould to obtain the light-weight rough blank of the water sports board.
16. The novel lightweight water sports board HEM molding process according to claim 11, wherein the fiber prepreg is composed of two layers of glass fiber prepreg cloth adjacent to the foam core material and one layer of 3k carbon fiber prepreg cloth outside the two layers of glass fiber prepreg cloth when the prepreg inclusion is prepared in step 3).
17. The novel lightweight water sports board HEM molding process according to claim 11, wherein when the fatigue test is performed on the water sports board blank, after 30000 reciprocations with a set force value of 50kg are performed at the middle position of the forefoot sleeve hole, the interface between the fiber composite material on the surface and the EEC foam core material inside the surface remains intact;
when the lateral bending resistance test is carried out on the rough blank of the water sports board, the water sports board is fixed on a vertical testing device, a flat bar (9) with the length of 850mm is fixed on a base (8), a 50kg weight (10) is hung on the top of the outer end of the flat bar, downward acting force is loaded by utilizing the weight dead weight, the bending test is carried out on the water sports board in two directions of the base respectively, and a fiber layer at the base and an internal foaming core material are kept intact;
when the stretching resistance test is carried out on the rough blank of the water sports board, the two ends of the water sports board are pressed near the middle part, the water sports board is stretched upwards from the base groove of the water sports board by a universal pulling machine, the stretching speed is 25mm/min, the stretching is stopped when the stretching force reaches 500kg, and the fiber layer of the base structure and the foaming core material inside are kept intact.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310057110.0A CN117551303A (en) | 2023-01-21 | 2023-01-21 | Novel light-weight water sports board HEM molding material and molding process |
| PCT/CN2023/078903 WO2024152411A1 (en) | 2023-01-21 | 2023-03-01 | New lightweight hem molding material for water sports board and molding process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310057110.0A CN117551303A (en) | 2023-01-21 | 2023-01-21 | Novel light-weight water sports board HEM molding material and molding process |
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| JP5513804B2 (en) * | 2009-08-06 | 2014-06-04 | テクノポリマー株式会社 | Thermoplastic resin composition for foam molding and foam molded body using the same |
| CN104448323B (en) * | 2014-12-18 | 2017-01-11 | 江苏美思德化学股份有限公司 | Starlike pectinate polyether-organosilicone copolymer and preparation method thereof |
| JP6839295B2 (en) * | 2016-10-11 | 2021-03-03 | アルコン インク． | Polymerizable Polydimethylsiloxane-Polyoxyalkylene Block Copolymer |
| CN113004524B (en) * | 2019-12-20 | 2023-01-13 | 万华化学集团股份有限公司 | Epoxy-organic silicon resin and preparation method and application thereof |
| CN113004523B (en) * | 2019-12-20 | 2022-08-05 | 万华化学集团股份有限公司 | Epoxy-organic silicon resin and preparation method and application thereof |
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