CN115489043A - Intermittent vacuum mechanical premixing method for resin-based premix - Google Patents
Intermittent vacuum mechanical premixing method for resin-based premix Download PDFInfo
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- CN115489043A CN115489043A CN202211417455.4A CN202211417455A CN115489043A CN 115489043 A CN115489043 A CN 115489043A CN 202211417455 A CN202211417455 A CN 202211417455A CN 115489043 A CN115489043 A CN 115489043A
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- 238000000034 method Methods 0.000 title claims abstract description 53
- 229920005989 resin Polymers 0.000 title claims abstract description 37
- 239000011347 resin Substances 0.000 title claims abstract description 37
- 239000000835 fiber Substances 0.000 claims abstract description 108
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000005011 phenolic resin Substances 0.000 claims abstract description 52
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 52
- 238000004898 kneading Methods 0.000 claims abstract description 48
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 21
- 230000008569 process Effects 0.000 claims abstract description 17
- 238000005303 weighing Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 54
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 49
- 229910021529 ammonia Inorganic materials 0.000 claims description 31
- 239000000203 mixture Substances 0.000 claims description 27
- 239000000377 silicon dioxide Substances 0.000 claims description 25
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- -1 phenolic aldehyde Chemical class 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 13
- 239000010453 quartz Substances 0.000 claims description 12
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 229910052749 magnesium Inorganic materials 0.000 claims description 10
- 239000011777 magnesium Substances 0.000 claims description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 4
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical compound [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229920006231 aramid fiber Polymers 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002131 composite material Substances 0.000 description 27
- 238000010438 heat treatment Methods 0.000 description 15
- 238000002360 preparation method Methods 0.000 description 10
- 239000004760 aramid Substances 0.000 description 9
- 229920003235 aromatic polyamide Polymers 0.000 description 9
- 239000003365 glass fiber Substances 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 2
- 239000006259 organic additive Substances 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000009489 vacuum treatment Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/002—Methods
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The invention relates to a resin-based premix intermittent vacuum mechanical premixing method; the method comprises the following steps: weighing a certain amount of phenolic resin, adding the phenolic resin into a kneading machine, adding an organic auxiliary agent, putting a certain amount of chopped fibers into the kneading machine at least three times after the kneading machine rotates forwards for a certain time, closing a kneading machine cover after all the fibers are put into the kneading machine, alternately rotating forwards and standing the kneading machine, vacuumizing the kneading machine in the rotating forwards and standing processes, removing the organic auxiliary agent, and obtaining a resin-based premix after the rotating forwards and standing are finished; the kneader alternately rotates forwards and stands, the standing time is 5-60 times of the rotating time, and the times of the rotation and the standing alternately are 8-10 times.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to an intermittent vacuum mechanical premixing method for a resin-based premix.
Background
The resin-based premix is an intermediate material of a resin-based composite material. The traditional chopped fiber/phenolic aldehyde premix production process is a manual premixing method. The manual premixing process has the defects of high labor intensity, low production efficiency, high labor cost, correlation between product quality and operator proficiency, large dispersion of resin content of the premix and the like.
Therefore, in view of the above problems, the present invention is urgently needed to provide a batch type vacuum mechanical premixing method for resin-based premixes.
Disclosure of Invention
The invention aims to provide a resin-based premix intermittent vacuum mechanical premixing method, which solves the technical problems of high labor intensity, low production efficiency, high labor cost, high premix resin content dispersion and the like of the prior art that a chopped fiber/phenolic premix production process is a manual premixing method. The invention provides a resin-based premix intermittent vacuum mechanical premixing method, which comprises the following steps:
weighing a certain amount of phenolic resin, adding the phenolic resin into a kneading machine, adding an organic auxiliary agent, positively rotating the kneading machine for a certain time, then adding a certain amount of chopped fibers into the kneading machine at least three times, closing a cover of the kneading machine after all the fibers are put into the kneading machine, alternately positively rotating and standing the kneading machine, vacuumizing the kneading machine in the processes of positively rotating and standing to remove the organic auxiliary agent, and obtaining a resin-based premix after the positively rotating and standing are finished;
wherein, the kneader alternately carries out forward rotation and standing, the standing time is 5-60 times of the forward rotation time, and the times of the alternate forward rotation and standing are 8-10 times.
Preferably, a certain amount of chopped fibers are fed into the kneader at least three times, and the kneader is rotated forward for 30 to 60 seconds after each feeding of chopped fibers.
Preferably, the addition amount of the organic auxiliary agent is 10-35% of the mass of the phenolic aldehyde.
Preferably, the mass ratio of the phenolic resin to the chopped fibers is (1-5): 2.
preferably, the obtained resin-based premix is subjected to tearing-loosening treatment, air-cured at room temperature for 2-3h, dried at 80-100 ℃ for 10min, and sealed for storage.
Preferably, in the batch type vacuum mechanical premixing process, the kneader alternately rotates forwards and stands, the forward rotation time of the kneader is 35-120s, and the standing time is 15-30min.
Preferably, the chopped fibres have a length of 30-50mm.
Preferably, the phenolic resin is one or a mixture of ammonia phenolic resin, magnesium phenolic resin, barium phenolic resin, boron-silicon phenolic resin, epoxy modified phenolic resin, benzoxazine resin, inorganic modified phenolic resin and nano modified phenolic resin.
Preferably, the organic auxiliary agent is one of absolute ethyl alcohol, acetone, butanone, petroleum ether or ethyl acetate.
Preferably, the chopped fiber is one or more of alkali-free glass chopped fiber, high silica chopped fiber, high-strength glass chopped fiber, alumina chopped fiber, aramid fiber chopped fiber, quartz chopped fiber and polyarylsulfone chopped fiber.
Preferably, a certain amount of phenolic resin is weighed and added into a kneader, an organic auxiliary agent is added, and in the process that the kneader rotates forwards for a certain time, the forward rotation time of the kneader is inversely proportional to the number of hydroxyl groups or/and the number of carboxyl groups contained in the phenolic resin;
in the process that the kneader alternately rotates forwards and stands, the forward rotation time of the kneader is inversely proportional to the number of hydroxyl groups or/and the number of carboxyl groups contained in the fiber.
Compared with the prior art, the intermittent vacuum mechanical premixing method for the resin-based premix provided by the invention has the following advantages:
1. the invention adopts intermittent vacuum mechanical mixing, kneads in a short time in a plurality of cycles, and stands for a long time in the middle, thus not only being capable of leading the fiber to be completely soaked by the resin, but also being capable of ensuring the uniformity of the premix, and also being capable of avoiding the problems of long fiber damage and the reduction of the strength of the premix caused by the over-kneading time.
2. The invention adopts vacuum mechanical premixing, and after multi-period kneading, fine treatment for removing organic additives is carried out in the vacuum treatment process, so that the uniformity of the gel content of the premix when the premix is taken out of a pot and aired can be ensured.
3. The invention adopts an intermittent vacuum mechanical premixing method, and compared with a manual premixing method, the number of operators can be reduced by more than 70%.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides a resin-based premix intermittent vacuum mechanical premixing method, which comprises the following steps:
weighing a certain amount of phenolic resin, adding the phenolic resin into a kneading machine, adding an organic auxiliary agent, positively rotating the kneading machine for a certain time, then adding a certain amount of chopped fibers into the kneading machine at least three times, closing a cover of the kneading machine after all the fibers are put into the kneading machine, alternately positively rotating and standing the kneading machine, vacuumizing the kneading machine in the processes of positively rotating and standing to remove the organic auxiliary agent, and obtaining a resin-based premix after the positively rotating and standing are finished;
wherein, the kneader alternately carries out forward rotation and standing, the standing time is 5-60 times of the forward rotation time, and the times of the alternate forward rotation and standing are 8-10 times.
Specifically, a certain amount of chopped fibers are fed into the kneader at least three times, and after each feeding of the chopped fibers, the kneader is rotated forward for 30 to 60 seconds.
The material is thrown many times, throw the material evenly, surely do not have the bold or increase the input suddenly, cause the fibre to be broken by machinery, and physical strength seriously descends, also prevents to mix the oar, mixes and receive inhomogeneous extrudability impact between the jar, causes the severity of equipment structural strength to destroy, even takes place "card oar" phenomenon.
Specifically, the addition amount of the organic auxiliary agent is 10-35% of the mass of the phenolic aldehyde.
Specifically, the mass ratio of the phenolic resin to the chopped fibers is (1-5): 2.
specifically, the obtained resin-based premix is subjected to tearing and loosening treatment, dried at room temperature for 2-3h, dried at 80-100 ℃ for 10min, and sealed for storage.
Specifically, in the batch type vacuum mechanical premixing process, the kneader alternately rotates forwards and stands, the forward rotation time of the kneader is 35-120s, and the standing time is 15-30min.
Specifically, the chopped fibers have a length of 30 to 50mm.
Specifically, the phenolic resin is one or a mixture of ammonia phenolic resin, magnesium phenolic resin, barium phenolic resin, boron-silicon phenolic resin, epoxy modified phenolic resin, benzoxazine resin, inorganic modified phenolic resin and nano modified phenolic resin.
Specifically, the organic auxiliary agent is one of absolute ethyl alcohol, acetone, butanone, petroleum ether or ethyl acetate.
Specifically, the chopped fibers are one or more of alkali-free glass fiber chopped fibers, high-silica chopped fibers, high-strength glass fiber chopped fibers, alumina chopped fibers, aramid fiber chopped fibers, quartz chopped fibers and polyarylsulfone chopped fibers.
Specifically, a certain amount of phenolic resin is weighed and added into a kneader, an organic auxiliary agent is added, and in the process that the kneader rotates forwards for a certain time, the forward rotation time of the kneader is inversely proportional to the number of hydroxyl groups or/and the number of carboxyl groups contained in the phenolic resin;
in the process that the kneader alternately rotates forwards and stands, the forward rotation time of the kneader is inversely proportional to the number of hydroxyl groups or/and the number of carboxyl groups contained in the fiber.
Specifically, the kneading machine is a vacuum kneading machine, stirring paddles of the vacuum kneading machine are sigma-shaped and are unfolded according to Archimedes spiral lines, the two stirring paddles are arranged in parallel and rotate oppositely and have different rotating speeds when in work, and the stirring paddles extrude the material in the axial direction and the radial direction, namely extrude the material at a high speed and extrude the material at a low speed; the squeezing movement and the separating movement are carried out. The parameters of the vacuum kneader are shown in Table 10.
The invention adopts intermittent vacuum mechanical mixing, kneads in a multi-cycle short time, and stands for a long time in the middle, so that the fiber can be completely soaked by the resin, the uniformity of the premix can be ensured, and the problems of long fiber damage and premix strength reduction caused by over-kneading time can be avoided.
The invention adopts vacuum mechanical premixing, and after multi-period kneading, fine treatment for removing organic additives is carried out in the vacuum treatment process, so that the gradient change of the gel content can be avoided when the premix is taken out of a pot and aired.
Compared with a manual premixing method, the invention adopts an intermittent vacuum mechanical premixing method, and the number of operators can be reduced by more than 70%.
Example one
The preparation process of the high silica chopped fiber/ammonia phenolic aldehyde premix (A1 premix) comprises the following steps:
101 Filtering the ammonia phenolic resin with a 100-200 mesh copper or stainless steel screen;
102 Cutting the high silica fiber into a length of 32mm, and drying in an oven at the drying temperature of 120 ℃ for 4h;
103 Weighing 35.5kg of ammonia phenolic resin, pouring into a 300L kneader, adding 15L of absolute ethyl alcohol, and positively rotating for 1min;
104 Adding 45kg of high silica fiber in three times, preferably uniformly adding 15kg of high silica fiber at each position of a kneader, rotating forward for 30s, adding 15kg of yarn uniformly, rotating forward for 30s, adding the rest 15kg of yarn uniformly, and closing a kneader cover;
105 Vacuum mechanical premixing, kneading eight times and standing eight times, vacuumizing the kneader at the same time, removing absolute ethyl alcohol, kneading for time and standing for time according to the table 1 to obtain a mixture;
106 Tearing and loosening the mixture twice by using a tearing and loosening machine, uniformly laying the mixture on a net grate, airing the mixture at room temperature for 2 hours, and drying the mixture in an oven at 80 ℃ for 10min to obtain a high-silica chopped fiber/ammonia phenolic aldehyde premix (A1 premix);
107 Testing the three-phase index of the A1 premix (the three-phase index of the A1 premix is shown in table 6), bagging and sealing after the product is qualified, and starting the A1 premix after three days.
The addition amount of the organic auxiliary agent is 33.3 percent of the mass of the ammonia phenolic resin.
The mass ratio of the amino phenolic resin to the high-silica chopped fibers is 1.6.
Preparation of high silica chopped fiber/Ammonia phenolic composite (composite B1)
108 Heating a mould to 80 ℃, filling the premix A1 into the mould, heating the mould to 100 ℃ within 50min, adding full pressure to 40MPa, deflating for 3 times before pressurizing, heating to 150 ℃ at the speed of 5 ℃/10min, preserving heat for 2min/mm, and naturally cooling to 60 ℃ to obtain the composite material B1, wherein the mechanical properties of the composite material B1 are shown in Table 10.
Example two
The preparation process of the high-silica chopped fiber/magnesium phenolic resin premix (A2 premix) comprises the following steps:
201 Filtering the magnesium phenolic resin with a 100-200 mesh copper or stainless steel screen;
202 Cutting the high silica fiber to a length of 50mm, and drying in an oven at a drying temperature of 120 ℃ for 4h;
203 47kg of magnesium phenolic resin is weighed and poured into a 300L kneader, 18L of acetone is added, and the mixture is positively rotated for 1min;
204 45kg of high silica fibers are added in three times, firstly 15kg of high silica fibers are evenly added at each position of a kneader, the mixture is rotated positively for 30s, then 15kg of yarns are evenly added, the mixture is rotated positively for 30s, the rest 15kg of yarns are evenly added, and a kneader cover is closed;
205 Vacuum mechanical premixing is carried out for eight times of kneading and eight times of standing, meanwhile, the kneader is vacuumized, acetone is removed, and kneading time and standing time are carried out according to the table 2, so as to obtain a mixture;
206 The mixture is torn loose twice by a tearing-loosening machine, evenly laid on a mesh, aired at room temperature for 2 hours, and dried in an oven at 80 ℃ for 10min to obtain high-silica chopped fiber/magnesium phenolic resin premix (A2 premix);
207 Testing the three-phase index of the A2 premix (the three-phase index of the A2 premix is shown in table 6), bagging and sealing after being qualified, and starting the A2 premix after three days.
The addition amount of the organic auxiliary agent is 30 percent of the mass of the ammonia phenolic resin.
The mass ratio of the magnesium phenolic resin to the high-silica chopped fibers is 1.04.
Preparation of high silica chopped fiber/magnesium phenolic composite (composite B2)
208 Heating the mold to 80 ℃, filling the A2 premix into the mold, heating the mold to 100 ℃ within 50min, adding full pressure to 40MPa, deflating for 3 times before pressurizing, heating to 150 ℃ at the speed of 5 ℃/10min, keeping the temperature for 2min/mm, and naturally cooling to 60 ℃ to obtain the composite material B2, wherein the mechanical properties are shown in Table 9.
EXAMPLE III
The preparation process of the quartz chopped fiber/ammonia phenolic aldehyde premix (A3 premix) comprises the following steps:
301 ) filtering the ammonia phenolic resin with a 100-200 mesh copper or stainless steel screen;
302 Cutting the quartz chopped fiber into a length of 32mm, and drying in an oven at the drying temperature of 120 ℃ for 4h;
303 41kg of ammonia phenolic resin is weighed and poured into a 300L kneader, 13L butanone is added, and the mixture rotates positively for 2min;
304 45kg of quartz chopped fibers are added in three times, firstly 15kg of quartz chopped fibers are evenly added into each position of a kneader and are positively rotated for 30s, then 15kg of quartz chopped fibers are evenly added and are positively rotated for 30s, the rest 15kg of quartz chopped fibers are evenly added, and a cover of the kneader is closed;
305 Vacuum mechanical premixing is carried out for eight times of kneading and eight times of standing, meanwhile, the kneader is vacuumized to remove butanone, and the kneading time and the standing time are carried out according to the table 3 to obtain a mixture;
306 Tearing and loosening the mixture twice by using a tearing and loosening machine, uniformly spreading the mixture on a mesh, airing the mixture at room temperature for 2 hours, and drying the mixture in an oven at 80 ℃ for 10min to obtain quartz chopped fiber/ammonia phenolic aldehyde premix (A3 premix);
307 Testing the three-phase index of the A3 premix (the three-phase index of the A3 premix is shown in table 6), bagging and sealing after being qualified, and starting the A3 premix after three days.
The addition amount of the organic auxiliary agent is 25 percent of the mass of the ammonia phenolic resin.
The mass ratio of the ammonia phenolic resin to the quartz chopped fibers is 1.8.
Preparation of Quartz chopped fiber/Ammonia phenolic composite Material (composite material B3)
308 Heating the mold to 80 ℃, loading the A3 premix into the mold, heating the mold to 100 ℃ within 50min, adding full pressure to 40MPa, deflating for 3 times before pressurizing, heating to 150 ℃ at the speed of 5 ℃/10min, keeping the temperature for 2min/mm, and naturally cooling to 60 ℃ to obtain the composite material B3, wherein the mechanical properties of the composite material B3 are shown in Table 9.
Example four
The preparation process of the aramid chopped fiber/ammonia phenolic aldehyde premix (A4 premix) comprises the following steps:
401 ) filtering the ammonia phenolic resin with a 100-200 mesh copper or stainless steel screen;
402 Cutting the aramid chopped fiber to a length of 30mm, and drying in an oven at a drying temperature of 120 ℃ for 4h;
403 55kg of ammonia phenolic resin is weighed and poured into a 500L kneader, 27L of petroleum ether is added, and positive rotation is carried out for 2min;
404 45kg of aramid chopped fibers are added in three times, firstly 15kg of aramid chopped fibers are evenly added at each position of a kneader and are positively rotated for 30s, then 15kg of aramid chopped fibers are evenly added and positively rotated for 30s, the rest 15kg of aramid chopped fibers are evenly added, and a kneader cover is closed;
405 Vacuum mechanical premixing, kneading eight times and standing eight times, vacuumizing the kneader to remove petroleum ether, and kneading for time and standing time according to the table 4 to obtain a mixture;
406 Tearing and loosening the mixture twice by using a tearing and loosening machine, uniformly spreading the mixture on a mesh, airing the mixture at room temperature for 2 hours, and drying the mixture in an oven at 80 ℃ for 10min to obtain aramid chopped fiber/ammonia phenolic aldehyde premix (A4 premix);
407 Testing A4 premix three-phase index (see Table 6 for A4 premix three-phase index), bagging and sealing after being qualified, and starting A4 premix after three days.
The addition amount of the organic auxiliary agent is 32 percent of the mass of the ammonia phenolic resin.
The mass ratio of the amino phenolic resin to the aramid chopped fibers is 2.4.
Preparation of aramid chopped fiber/Ammonia phenolic composite material (composite material B4)
408 Heating the mold to 80 ℃, loading the A4 premix into the mold, heating the mold to 100 ℃ within 50min, adding full pressure to 40MPa, deflating for 3 times before pressurizing, heating to 150 ℃ at the speed of 5 ℃/10min, keeping the temperature for 2min/mm, and naturally cooling to 60 ℃ to obtain the composite material B4, wherein the mechanical properties of the composite material B4 are shown in Table 9.
EXAMPLE five
The preparation process of the high silica fiber and high strength glass fiber chopped fiber compound fiber/ammonia phenolic aldehyde premix (A5 premix) comprises the following steps:
501 ) filtering the ammonia phenolic resin with a 100-200 mesh copper or stainless steel screen;
502 Cutting the high-silica fiber and the high-strength glass fiber into short fibers with the cutting length of 32mm, and drying in an oven at the drying temperature of 120 ℃ for 4 hours;
503 42kg of ammonia phenolic resin is weighed and poured into a 500L kneader, 10L of ethyl acetate is added, and the mixture is positively rotated for 2min;
504 Adding 45kg of the high silica fiber and high-strength glass fiber chopped fiber compound fiber in three times, firstly uniformly adding 15kg of the compound fiber into each part of a kneading machine, rotating forward for 30s, then uniformly adding 15kg of the compound fiber, rotating forward for 30s, uniformly adding the rest 15kg of the compound fiber, and closing a cover of the kneading machine;
505 Vacuum mechanical premixing, kneading eight times and standing eight times, vacuumizing the kneader, removing ethyl acetate, and kneading and standing for the time shown in Table 4 to obtain a mixture;
506 The mixture is torn loose twice by a tearing and loosening machine, evenly laid on a mesh, dried for 2 hours at room temperature, and dried for 10min in an oven at 80 ℃ to obtain the high silica fiber and high-strength glass fiber chopped fiber compound fiber/ammonia phenolic premix (A5 premix);
507 Testing A5 premix three-phase index (see Table 6 for A5 premix three-phase index), bagging and sealing after being qualified, and starting the A5 premix after three days.
The addition amount of the organic auxiliary agent is 21 percent of the mass of the ammonia phenolic resin.
The mass ratio of the ammonia phenolic resin to the high silica fiber to the high-strength glass fiber chopped fiber compound fiber is 1.9.
High silica fiber and high strength glass fiber chopped fiber composite fiber/ammonia phenolic composite material (composite material B5)
508 Heating the mold to 80 ℃, filling the A5 premix into the mold, heating the mold to 100 ℃ within 50min, adding full pressure to 40MPa, deflating for 3 times before pressurizing, heating to 150 ℃ at the speed of 5 ℃/10min, preserving heat for 2min/mm, and naturally cooling to 60 ℃ to obtain the composite material B5, wherein the mechanical properties of the composite material B5 are shown in Table 9.
Comparative example 1
The high silica chopped fiber/ammonia phenolic aldehyde premix (C1 premix) is prepared by a manual premixing method, the proportion of the C1 premix and the mould pressing process of the composite material are the same as those in the embodiment 1, three indexes of the C1 premix are shown in a table 6, and the D1 of the composite material obtained by the C1 premix is shown in a table 9.
Comparative example 2
The high silica chopped fiber/magnesium phenolic aldehyde premix (C2 premix) is prepared by a manual premixing method, the proportioning of the C2 premix and the mould pressing process of the composite material are the same as those of the embodiment 2, three indexes of the C2 premix are shown in a table 6, and a composite material D2 obtained by the C2 premix is shown in a table 9.
Compared with comparative example 1 and comparative example 2, under the condition of the same production capacity, the number of workers is reduced by over 70%, the production time is greatly shortened, the total working hours are short, and the production efficiency is improved by 7.2 times.
The resin content uniformity of the premix prepared by the batch vacuum mechanical premixing method is better than that of the manual premixing method, and the dispersion coefficients in the example I and the example II are far lower than those in the comparative example 1 and the comparative example 2.
The mechanical properties of the composite material obtained by the mould pressing of the premix prepared by the intermittent vacuum mechanical premixing method and the manual premixing method are equivalent.
The premix prepared by the intermittent vacuum mechanical premixing method has uniform gel content.
The invention adopts intermittent vacuum mechanical mixing, kneads in a short time in a plurality of cycles, and stands for a long time in the middle, thus not only being capable of leading the fiber to be completely soaked by the resin, but also being capable of ensuring the uniformity of the premix, and also being capable of avoiding the problems of long fiber damage and the reduction of the strength of the premix caused by the over-kneading time.
TABLE 1 intermittent vacuum mechanical premixing
TABLE 2 intermittent vacuum mechanical premixing
TABLE 3 intermittent vacuum mechanical premixing
TABLE 4 batch vacuum mechanical premixing
TABLE 5 intermittent vacuum mechanical premixing
TABLE 6 preparation of premix by mechanical premixing method and manual premixing method
TABLE 7 coefficient of variation of resin content in the mechanically and manually premixed premixes
TABLE 8 comparison of working hours for mechanical and manual premixing processes
TABLE 9 mechanical Properties of the composites
TABLE 10 vacuum kneader parameters
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A resin-based premix intermittent vacuum mechanical premixing method is characterized in that: the method comprises the following steps:
weighing phenolic resin, adding the phenolic resin into a kneading machine, adding an organic auxiliary agent, putting chopped fibers into the kneading machine at least three times after the kneading machine rotates forwards, closing a kneading machine cover after all the fibers are put into the kneading machine, alternately rotating forwards and standing the kneading machine, vacuumizing the kneading machine in the rotating forwards and standing processes to remove the organic auxiliary agent, and obtaining a resin-based premix after the rotating forwards and standing are finished;
wherein the kneader alternately carries out forward rotation and standing, the standing time is 5-60 times of the forward rotation time, and the number of times of alternate forward rotation and standing is 8-10.
2. The intermittent vacuum mechanical premixing method for resin-based premixes of claim 1, wherein: and (3) feeding the chopped fibers into a kneader at least three times, and rotating the kneader forward for 30-60s after each time of feeding the chopped fibers.
3. The intermittent vacuum mechanical premixing method for resin-based premixes of claim 1, wherein: the addition amount of the organic auxiliary agent is 10-35% of the mass of the phenolic aldehyde.
4. The batch vacuum mechanical premixing method for the resin-based premix according to claim 1, wherein: the mass ratio of the phenolic resin to the chopped fibers is (1-5): 2.
5. the intermittent vacuum mechanical premixing method for resin-based premixes of claim 1, wherein: and (3) tearing and loosening the obtained resin-based premix, airing at room temperature for 2-3h, drying at 80-100 ℃ for 10min, and sealing and storing.
6. The intermittent vacuum mechanical premixing method for resin-based premixes of claim 1, wherein: in the intermittent vacuum mechanical premixing process, the kneader alternately performs forward rotation and standing, wherein the forward rotation time of the kneader is 35-120s, and the standing time is 15-30min.
7. The intermittent vacuum mechanical premixing method for resin-based premixes of claim 1, wherein: the length of the chopped fiber is 30-50mm.
8. The batch vacuum mechanical premixing method for the resin-based premix according to claim 1, wherein: the phenolic resin is one or a mixture of ammonia phenolic resin, magnesium phenolic resin, barium phenolic resin, boron-silicon phenolic resin, epoxy modified phenolic resin, benzoxazine resin, inorganic modified phenolic resin and nano modified phenolic resin.
9. The intermittent vacuum mechanical premixing method for resin-based premixes of claim 1, wherein: the organic auxiliary agent is one of absolute ethyl alcohol, acetone, butanone, petroleum ether or ethyl acetate.
10. The intermittent vacuum mechanical premixing method for resin-based premixes of claim 1, wherein: the chopped fiber is one or more of alkali-free glass chopped fiber, high-silica chopped fiber, high-strength glass chopped fiber, alumina chopped fiber, aramid fiber chopped fiber, quartz chopped fiber and polyarylsulfone chopped fiber.
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| CN113954257A (en) * | 2021-09-30 | 2022-01-21 | 北京元蛋复合材料有限公司 | Intermittent equidirectional vacuum mechanical premixing preparation method for aerospace ablation heat-proof chopped fiber/phenolic aldehyde premix |
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| JPH08283534A (en) * | 1995-04-20 | 1996-10-29 | Sumitomo Bakelite Co Ltd | Melamine-phenol resin composition |
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