CN116587511A - Preparation method of segmented foam material - Google Patents

Preparation method of segmented foam material Download PDF

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Publication number
CN116587511A
CN116587511A CN202310538042.XA CN202310538042A CN116587511A CN 116587511 A CN116587511 A CN 116587511A CN 202310538042 A CN202310538042 A CN 202310538042A CN 116587511 A CN116587511 A CN 116587511A
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CN
China
Prior art keywords
pressure
temperature
foaming
polymer
saturation
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Pending
Application number
CN202310538042.XA
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Chinese (zh)
Inventor
翁成龙
王镇
王佳林
钱家欢
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Zhejiang Xinhengtai New Materials Co ltd
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Zhejiang Xinhengtai New Materials Co ltd
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Priority to CN202310538042.XA priority Critical patent/CN116587511A/en
Publication of CN116587511A publication Critical patent/CN116587511A/en
Pending legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • 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
    • B29C44/08—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 using several expanding or moulding steps
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Abstract

The invention relates to the field of foaming materials, in particular to a preparation method of a sectional foaming material, which comprises the steps of firstly carrying out basic processing on the material, then adopting a high-pressure tank with higher pressure to carry out gas saturation, after the gas is completely saturated, decompressing at an extremely low decompression rate, simultaneously cooling, inducing the inside of a polymer to generate extremely small bubble nuclei through pressure reduction, wherein the bubble nuclei are origins of bubble generation, simultaneously improving the viscosity of the whole foaming material through the reduction of the outside air temperature, preventing the overflow of the inside high-pressure gas and the growth of the polymer material, then placing the saturated material in a molding press, wherein the inside of the molding press is in a high-temperature low-pressure state, the growth of cells is induced through temperature change, and the outside is blocked by pressure to avoid the rapid escape of the gas inside the material, so that the problem of lower foaming efficiency is avoided; the invention ensures that the foam cells of the obtained foaming material are fine and smooth and the rebound resilience is good, and the preparation process is efficient and quick.

Description

Preparation method of segmented foam material
Technical Field
The invention relates to the field of preparation methods of germinal foam materials, in particular to a preparation method of a segmented foam material.
Background
At present, the main means for preparing the polymer foaming material is still chemical foaming, and the chemical foaming is prepared by compounding a series of auxiliary agents with a chemical foaming agent, so that the polymer foaming material has absolute advantages in cost and efficiency, but along with the increasing strictness of environmental protection requirements, the preparation of the polymer foaming material by clean and nontoxic supercritical fluid is becoming the main stream guidance of the market.
The supercritical foaming technology commonly used in the market at present comprises three types of extrusion foaming, injection foaming and intermittent foaming. The extrusion foaming and injection foaming are carried out by utilizing melt to uniformly blend polymer and supercritical gas in the advancing process of a screw rod through screw rod shearing, and foaming is completed when the polymer and supercritical gas come out of a die. Compared with the two, the intermittent foaming has lower efficiency, but the obtained product has stable quality and fine foam cells, and is suitable for preparing the foaming material with larger size.
The supercritical foaming process needs to go through three stages of gas saturation, nucleation and bubble growth, wherein the gas saturation rate directly determines the production efficiency, the nucleation efficiency determines the cell density, and the bubble growth stage determines the cell diameter. The three stages of saturation-nucleation-growth of most batch foaming techniques are all in one mold cavity, for example, the modes mentioned in the application of the Chinese invention with publication number of CN112552546A and the Chinese invention with publication number of CN102167840B are all completed in one mold cavity, which results in that the mold cavity needs to be large when producing large-size foaming materials, high requirements are put on high-pressure gas sealing, the temperature is mostly lower than Tm, and the saturation efficiency is low. And CO is adopted for preparing the supercritical foaming material at present 2 As a foaming agent, due to CO 2 The very high permeation rate compared to air, and therefore, a large area shrinkage phenomenon occurs when some elastomer foaming materials are prepared, resulting in low quality of the finished product.
At present, intermittent foaming is interfered by a plurality of factors such as equipment, process, formula and the like, and some thermoplastic polymer foaming materials cannot be efficiently prepared.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is that the existing intermittent foaming is interfered by a plurality of factors such as equipment, process, formula and the like, and some thermoplastic polymer foaming materials cannot be efficiently prepared.
In order to solve the technical problems, the invention provides a preparation method of a segmented foam material, wherein the preparation method of the foam material adopts various base materials, is not only limited to TPU, but also comprises materials with common thermoplastic materials, crosslinked materials and partially crosslinked island structures, and the invention needs to perform basic processing on the materials, such as extrusion, foaming and the like, so as to prepare the materials into plates or special-shaped shapes for foaming; the foaming is carried out in a coupling mode of the high-pressure tank and the high-pressure press, namely, the high-pressure tank capable of achieving higher pressure is adopted for gas saturation, after the gas is completely saturated, the pressure is relieved at an extremely low pressure relief rate, the temperature is reduced, the interior of the polymer is induced to generate extremely small bubble nuclei through pressure reduction, the bubble nuclei are origins of bubble generation, the viscosity of the whole foaming material is improved through the reduction of the outside air temperature, the overflow of the high-pressure gas and the growth of the polymer material are prevented, then the saturated material is placed in the molding press, the inside of the molding press is in a high-temperature low-pressure state, the pressure is lower than the saturation pressure, the growth of cells is triggered through temperature change, and the pressure is blocked outside to prevent the gas in the material from escaping rapidly, so that the problem of lower foaming efficiency is avoided; according to the invention, the two processes of nucleation and growth of foaming are cut, the equipment size requirement in the foaming process is reduced firstly, the foaming can be induced through the temperature and pressure change of a coupled mould pressing foaming machine after the second nucleation, the foaming rate is more controllable, the high-pressure tank in the third nucleation process can provide higher pressure and temperature, and more polymer types can be adapted.
The two processes of nucleation and growth of foaming are cut and the saturated mother board is subjected to low-temperature treatment, so that local saturation and foaming in different places can be realized. The unfoamed mother board is transported in the first transportation process, so that the transportation cost of the foaming material can be greatly reduced; secondly, because the size of the unfoamed mother board is smaller, a plurality of mother boards can be saturated at one time in a high-pressure tank in the preamble process, and the size of the mother boards can be enlarged after foaming in a foaming machine (a molding press) in the preamble process, so that the number of the mother boards subjected to single foaming is smaller, if the storage time of the mother boards subjected to saturation is shorter, the time interval for waiting for foaming is shorter, and the mother boards subjected to the follow-up process are less in conflict with the single yield of the mother boards in the foaming machine, thereby being unfavorable for improving the production efficiency.
The method comprises the following steps:
1) Thermoplastic polymer particles are taken as a base material, various auxiliary agents are compounded, and a solid plate or a blank to be foamed of a special-shaped material is prepared through a forming process;
2) Placing the blank to be foamed in a one-stage autoclave for high-temperature high-pressure supercritical fluid saturation, wherein the supercritical fluid is N 2 The method comprises the steps of carrying out a first treatment on the surface of the If the blank to be foamed is a polymer without crosslinking, the saturation temperature is set at T g (glass transition temperature of Polymer) and T m (melting temperature of the polymer); if the blank to be foamed is a crosslinked or fully crosslinked polymer, setting the saturation temperature at T m The above;
3) After saturation, the pressure is reduced to a certain value, nucleation is carried out, the temperature of the autoclave is reduced to normal temperature, and the residual pressure is discharged after the temperature is reduced to normal temperature;
4) And (3) placing the nucleated material in the step (3) in a high-temperature low-pressure die again for foaming to obtain the foaming material.
Preferably, the thermoplastic polymer in step 1) may be one or more of the composites of PS, PP, PE, POE, OBCs, VISTAMAX, TPU, TPEE, PEBAX, EVA, EPDM, SEBS, PVDF.
Preferably, the molding process in step 1) may be extrusion, injection molding, hot pressing, 3D printing, and the like.
Preferably, the auxiliary agent in the step 1) comprises one or more of a cross-linking agent, a sensitizer, a nucleating agent, a color master, a flame retardant and an antistatic agent.
Preferably, the foamed blank in step 2) may be a non-crosslinked polymer, a partially crosslinked polymer or a fully crosslinked polymer.
Preferably, the saturation pressure in step 2) is > atmospheric pressure.
Preferably, the polymer saturated with gas in step 3) may be stored at 0 ℃ and below to extend its storage time.
Preferably, the depressurization rate in step 3) is from 0.1MPa/s to 20MPa/s, and the reduced pressure is from 1 to 8MPa.
Preferably, the high-temperature high-pressure die in the step 4) is a supercritical die pressing foaming machine, the temperature range is 100-200 ℃, and the pressure range is 1-16 MPa.
Preferably, the cross-linking mode of the cross-linked polymer can be chemical cross-linking or irradiation cross-linking, and the preparation mode of the partially cross-linked polymer is that the whole cross-linked polymer and the uncrosslinked polymer are melt blended.
The technical scheme of the invention has the following beneficial effects:
1. the invention adopts the mode of combining the autoclave and the molding press to foam, the gas saturation and the nucleation are carried out in the autoclave, the pressure is higher during the gas saturation, and then the nucleation is carried out by low-speed decompression, the volume of the blank to be foamed in the two stages is not large, so the volume of the autoclave is not required to be large, the sealing difficulty of the autoclave to high-pressure gas is small, the bubble growth is carried out in the molding press after the nucleation, because the growth of the bubble only needs to be low pressure, and the material to be foamed is generally cut into small pieces in the molding press, thereby the molding press does not need to consider the problem of high-pressure gas sealing. The invention can avoid the condition that the prior material to be foamed has higher requirement on the sealing performance of high-pressure gas because each stage of foaming is completed in the same die cavity;
2. the foaming material obtained by the preparation method has very small pore diameter and very large cell density due to high-pressure nucleation, and has very excellent rebound resilience;
3. selectively setting the saturation temperature between Tg and Tm when foaming the uncrosslinked polymer; when the polymer is foamed and partially crosslinked or fully crosslinked, the saturation temperature is set above Tm, the molecular chain spacing is widened, the saturation speed is increased, and the quantity of saturated gas is increased. And when the uncrosslinked polymer is saturated, the high-pressure tank can provide ultrahigh pressure compared with the traditional equipment, and the saturation speed and the saturated gas quantity can be increased.
4. The nucleated polymer saturated with high-pressure gas is placed in an environment at 0 ℃ or below 0 ℃, the precipitation of internal gas is slowed down, the process of local saturation and foaming in different places can be realized, the saturated polymer can be transported to other places for foaming, and the problem of high transportation cost of the foaming material is solved.
5. The nucleation and foaming are divided, so that the method has more operability in raw materials and processes. The equipment size requirement in the foaming process is reduced firstly, the foaming can be induced through the temperature and pressure change of a coupled mould pressing foaming machine after the second nucleation, the foaming rate is more controllable, the high-pressure tank in the third nucleation process can provide higher pressure and temperature, and more polymer types can be adapted.
6. The invention adopts N 2 Foaming and avoid due to CO 2 Compared with air, the air-permeable porous ceramic material has extremely high permeation rate, and the finished product has large area shrinkage.
Detailed Description
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between the two components. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
In addition, the technical features of the different embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Example 1: TPU is prepared by: the ratio of color masterbatch=95:5 is formed into a solid plate material with 1200 mm to 400 mm to 12mm by extrusion, the plate material is placed in a high-pressure tank, the saturation temperature is set at 130 ℃, and N is introduced 2 Reducing the pressure to 10MPa through a speed of 0.1MPa/s after saturation for 2 hours until the pressure reaches 22MPa, reducing the temperature of a high-pressure tank to normal temperature while initiating internal nucleation, discharging the residual pressure after the temperature is reduced to normal temperature, slightly expanding the saturated sheet to 1250 x 450 x 12.5mm, placing the saturated sheet in a molding press, setting the temperature of the molding press to 125 ℃, and setting the temperature of 2MPaN 2 And (5) foaming under pressure, and releasing the pressure to open the die after the foaming is finished to obtain the foaming TPU plate.
Example 2: preparing POE (polyolefin elastomer) into coiled material with width of 350mm and thickness of 2mm by extrusion casting, crosslinking the coiled material by irradiation with irradiation dose of 10Mev to obtain radiation crosslinked coiled material with gel content of 40%, and placing in a high-pressure tank for supercritical N 2 Soaking at 240 deg.c and 25MPa, saturating for 1 hr, lowering the pressure to 8MPa at 0.1MPa/s to initiate growth of inner bubble nucleus while lowering the temperature of the high pressure tank to room temperature, discharging the rest pressure fast after lowering the temperature to room temperature, changing the thickness of saturated coiled material to 2.2mm, increasing the width to 385mm, cutting the sheet material into 1300 x 385 x 2.5mm sheet material, stacking, placing in supercritical molding foaming machine at 160 deg.c and 3MPa N 2 Foaming is carried out under pressure, and after foaming is finished, the die is opened, the pressure is relieved, and the die is opened, so that the foaming POE sheet is obtained.
Example 3: EPDM: DCP: znst=100:1: 0.5 is put into an internal mixer for internal mixing and crosslinking (DCP is a crosslinking agent, znSt is a lubricant), the temperature is 150 ℃ and the time is 12min, so that the crosslinked EPDM material with the gel content of 30% is obtained, the crosslinked EPDM material is crushed into particles of 0.2mm by a particle crusher, and then the uncrosslinked EPDM material is extruded by an extruder: crosslinking epdm=80:20 to obtain a composite EPDM unfoamed sheet with "islands-in-the-sea" structure, 5mm in size 1150 x 200 x 5mm, and placing it in a high pressure tank for supercritical N 2 Impregnating at 100 deg.C and 18MPa, and saturating3h later, the internal bubble nucleus growth is initiated by reducing the pressure to 4MPa at the speed of 0.1MPa/s, the temperature of a high-pressure tank is reduced to room temperature, the residual pressure is rapidly discharged after the temperature is reduced to room temperature, the size of the sheet material is changed to 1180 x 205 x 5.1mm, the sheet material is taken out after being placed at 0 ℃ for 24h, the sheet material is placed in a supercritical die pressing foaming machine, the die pressing foaming machine temperature is set to be 100 ℃, and the pressure of 3MPa N 2 Foaming is carried out under pressure, and after foaming is finished, the die is opened, the pressure is relieved, and the die is opened, so that the foaming EPDM sheet is obtained.
Comparative example 1: TPU is prepared by: the ratio of color masterbatch=95:5 is formed into a solid plate with 1200 mm to 400 mm to 12mm by extrusion, the plate is placed in a supercritical die pressing foaming machine, the temperature of the pressing machine is set to 125 ℃, and the temperature of the pressing machine is set to 14MPa N 2 Saturated for 6 hours under pressure, rapidly depressurized and foamed to obtain the foamed TPU plate.
Comparative example 2: TPU is prepared by: the ratio of color masterbatch=95:5 is formed into a solid plate material with 1200 mm to 400 mm to 12mm by extrusion, the plate material is placed in a high-pressure tank, the saturation temperature is set at 130 ℃, and N is introduced 2 And (3) after the mixture is saturated for 2 hours at 22MPa, the pressure is reduced to normal pressure through the speed of 10MPa/s to initiate internal nucleation and foaming, and the foaming TPU plate is obtained.
Comparative example 3: preparing POE into coiled material with width of 350mm and thickness of 2mm by extrusion casting, and placing in a high-pressure tank for supercritical N 2 Soaking at 240 deg.c and 25MPa, saturating for 1 hr, lowering the pressure to 8MPa at 0.1MPa/s to initiate growth of inner bubble nucleus while lowering the temperature of the high pressure tank to room temperature, discharging the rest pressure fast after lowering the temperature to room temperature, changing the thickness of saturated coiled material to 2.2mm, increasing the width to 385mm, cutting the sheet material into 1300 x 385 x 2.5mm sheet material, stacking, placing in supercritical molding foaming machine at 160 deg.c and 3MPa N 2 Foaming is carried out under pressure, and after foaming is finished, the die is opened, the pressure is relieved, and the die is opened, so that the foaming POE sheet is obtained.
Comparative example 4: EPDM: DCP: znst=100:1: 0.5 is put into an internal mixer to carry out internal mixing and crosslinking (DCP is a crosslinking agent, znSt is a lubricant), the temperature is 150 ℃ and the time is 12min, and the crosslinked EPDM material with 30 percent of gel content is obtained through granular powderThe chopper crushed it to 0.2mm particles, followed by extrusion of the uncrosslinked EPDM through the extruder: crosslinking epdm=80:20 to obtain a composite EPDM unfoamed sheet with "islands-in-the-sea" structure, 5mm in size 1150 x 200 x 5mm, and placing it in a high pressure tank for supercritical N 2 Soaking at 100deg.C, saturated pressure of 18MPa, saturated for 3 hr, reducing pressure to 4MPa at 0.1MPa/s to induce growth of internal bubble nuclei while maintaining high pressure tank temperature to room temperature, rapidly discharging the rest pressure after temperature is reduced to room temperature, changing plate size to 1180 x 205 x 5.1mm sheet, standing at room temperature, taking out for 24 hr, standing in supercritical compression molding foaming machine, setting the temperature of compression molding foaming machine at 100deg.C, and 3MPa N 2 Foaming is carried out under pressure, and after foaming is finished, the die is opened, the pressure is relieved, and the die is opened, so that the foaming EPDM sheet is obtained.
Test data

Claims (10)

1. The preparation method of the segmented foam material is characterized by comprising the following steps of:
1) Thermoplastic polymer particles are taken as a base material, various auxiliary agents are compounded, and a solid plate or a blank to be foamed of a special-shaped material is prepared through a forming process;
2) Placing the blank to be foamed in a one-stage autoclave for high-temperature high-pressure supercritical fluid saturation, wherein the supercritical fluid is N 2 The method comprises the steps of carrying out a first treatment on the surface of the If the blank to be foamed is a polymer without crosslinking, the saturation temperature is set at T g (glass transition temperature of Polymer) and T m (melting temperature of the polymer); if the blank to be foamed is a crosslinked or fully crosslinked polymerSetting the saturation temperature at T m The above;
3) After saturation, the pressure is reduced to a certain value, nucleation is carried out, the temperature of the autoclave is reduced to normal temperature, and the residual pressure is discharged after the temperature is reduced to normal temperature;
4) And (3) placing the nucleated material in the step (3) in a high-temperature low-pressure die again for foaming to obtain the foaming material.
2. The method of claim 1, wherein the thermoplastic polymer in step 1) is one or more of PS, PP, PE, POE, OBCs, VISTAMAX, TPU, TPEE, PEBAX, EVA, EPDM, SEBS, PVDF.
3. The method for preparing the segmented foam material according to claim 1, wherein the molding process in the step 1) can be extrusion, injection molding, hot pressing, 3D printing and the like.
4. The method for preparing the segmented foam material according to claim 1, wherein the auxiliary agent in the step 1) comprises one or more of a crosslinking agent, a sensitizer, a nucleating agent, a color master, a flame retardant and an antistatic agent.
5. The method of claim 1, wherein the foamed blank in step 2) is a non-crosslinked polymer, a partially crosslinked polymer, or a fully crosslinked polymer.
6. The method for producing a segmented foam according to claim 1, wherein the saturation pressure in step 2) is > atmospheric pressure.
7. The method of producing a segmented foam according to claim 1, wherein the polymer saturated with gas in step 3) can be stored at 0 ℃ or below to extend the storage time.
8. The method for producing a segmented foam according to claim 1, wherein the depressurization rate in step 3) is 0.1MPa/s to 20MPa/s, and the reduced pressure is 1 to 10MPa.
9. The method for preparing a segmented foam material according to claim 1, wherein the high-temperature high-pressure die in the step 4) is a supercritical compression molding foaming machine, the temperature range is 100-200 ℃, and the pressure range is 1-16 MPa.
10. The method for preparing the segmented foam material according to claim 1, wherein the crosslinking mode of the crosslinked polymer is chemical crosslinking or irradiation crosslinking, and the preparation mode of the partially crosslinked polymer is melt blending of all crosslinked polymers and uncrosslinked polymers.
CN202310538042.XA 2023-05-15 2023-05-15 Preparation method of segmented foam material Pending CN116587511A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310538042.XA CN116587511A (en) 2023-05-15 2023-05-15 Preparation method of segmented foam material

Publications (1)

Publication Number Publication Date
CN116587511A true CN116587511A (en) 2023-08-15

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Application Number Title Priority Date Filing Date
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