CN118063890A - PP (Polypropylene) physical micro-foaming diffusion plate and manufacturing method thereof - Google Patents
PP (Polypropylene) physical micro-foaming diffusion plate and manufacturing method thereof Download PDFInfo
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- 238000009792 diffusion process Methods 0.000 title claims abstract description 60
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 36
- 238000005187 foaming Methods 0.000 title claims abstract description 24
- -1 Polypropylene Polymers 0.000 title claims abstract description 17
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 239000011256 inorganic filler Substances 0.000 claims abstract description 32
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 20
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 14
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 14
- 239000000314 lubricant Substances 0.000 claims abstract description 14
- 239000002667 nucleating agent Substances 0.000 claims abstract description 14
- 239000006260 foam Substances 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 57
- 239000000463 material Substances 0.000 claims description 51
- 238000003756 stirring Methods 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 35
- 239000002091 nanocage Substances 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 239000002243 precursor Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 15
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims description 15
- 229910052573 porcelain Inorganic materials 0.000 claims description 15
- 238000001125 extrusion Methods 0.000 claims description 14
- 239000012621 metal-organic framework Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000003892 spreading Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 8
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 8
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- KOUDKOMXLMXFKX-UHFFFAOYSA-N sodium oxido(oxo)phosphanium hydrate Chemical compound O.[Na+].[O-][PH+]=O KOUDKOMXLMXFKX-UHFFFAOYSA-N 0.000 claims description 6
- 229940026189 antimony potassium tartrate Drugs 0.000 claims description 5
- WBTCZEPSIIFINA-MSFWTACDSA-J dipotassium;antimony(3+);(2r,3r)-2,3-dioxidobutanedioate;trihydrate Chemical compound O.O.O.[K+].[K+].[Sb+3].[Sb+3].[O-]C(=O)[C@H]([O-])[C@@H]([O-])C([O-])=O.[O-]C(=O)[C@H]([O-])[C@@H]([O-])C([O-])=O WBTCZEPSIIFINA-MSFWTACDSA-J 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 230000003068 static effect Effects 0.000 claims description 5
- 238000011144 upstream manufacturing Methods 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical group N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000002347 injection Methods 0.000 abstract description 2
- 239000007924 injection Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- NNWPJQJICQTQOJ-UHFFFAOYSA-N O.[Na+].[Na+].[Na+].[O-]P([O-])[O-] Chemical compound O.[Na+].[Na+].[Na+].[O-]P([O-])[O-] NNWPJQJICQTQOJ-UHFFFAOYSA-N 0.000 description 6
- YPMOSINXXHVZIL-UHFFFAOYSA-N sulfanylideneantimony Chemical compound [Sb]=S YPMOSINXXHVZIL-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- IIQJBVZYLIIMND-UHFFFAOYSA-J potassium;antimony(3+);2,3-dihydroxybutanedioate Chemical compound [K+].[Sb+3].[O-]C(=O)C(O)C(O)C([O-])=O.[O-]C(=O)C(O)C(O)C([O-])=O IIQJBVZYLIIMND-UHFFFAOYSA-J 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical group CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000002666 chemical blowing agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000012994 photoredox catalyst Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
-
- 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
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/122—Hydrogen, oxygen, CO2, nitrogen or noble gases
-
- 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
- C08J9/0066—Use of inorganic compounding ingredients
-
- 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
- C08J9/0066—Use of inorganic compounding ingredients
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
-
- 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
- C08J9/009—Use of pretreated compounding ingredients
-
- 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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
-
- 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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/08—Supercritical fluid
-
- 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
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention relates to the technical field of diffusion plates, in particular to a PP physical micro-foaming diffusion plate and a manufacturing method thereof, which are prepared from the following raw materials in parts by weight: 100-120 parts of polypropylene, 1-3 parts of light diffusion agent master batch, 2-7 parts of nucleating agent, 20-30 parts of inorganic filler, 0.2-1.0 part of antioxidant and 1-2 parts of lubricant. According to the micro-foaming diffusion plate, the prepared inorganic filler is added into the polypropylene matrix, and foam holes which are uniformly distributed and basically consistent in size and aperture are formed in the diffusion plate in a supercritical nitrogen injection mode, so that the uniformity of foam cores is realized, and a better light diffusion effect can be achieved.
Description
Technical Field
The invention relates to the technical field of diffusion plates, in particular to a PP physical micro-foaming diffusion plate and a manufacturing method thereof.
Background
The light diffusion plate is characterized in that the light diffusion plate utilizes the physical phenomena of refraction, reflection and scattering when light encounters two mediums with different refractive indexes in the way of traveling through chemical or physical means, and inorganic or organic light diffusion agents are added in the base materials such as PMMA, PC, PS, PP or the like, or the light is artificially regulated through the array arrangement of micro-feature structures on the surface of the base materials, so that the light is refracted, reflected and scattered in different directions, the traveling route of the light is changed, the effect of fully dispersing the incident light to generate optical diffusion is realized, and the light diffusion plate is widely applied to liquid crystal display, LED illumination and imaging display systems.
For example, the invention patent publication No. CN113150357A discloses a method for manufacturing a closed cell micro-foaming diffusion plate, wherein raw materials, hydrocerol chemical foaming agent, flame retardant and diffusion agent are fully mixed; heating the mixture to a preset temperature T1, and conveying the mixture to the feeding end of the multistage gradient extrusion roller through a plurality of spiral conveying machines which are arranged side by side in parallel; cooling a diffusion plate extruded from the discharge end of the multistage gradient extrusion roller; cutting the edge of the diffusion plate when the temperature of the diffusion plate is reduced to a preset temperature T2; the multistage gradient squeeze rollers comprise a plurality of pairs of squeeze rollers which are arranged side by side and sequentially reduce the roller spacing; ; chemical blowing agents hydrocerol are used, which are compounds that release gases upon thermal decomposition, and which are capable of forming pores in the polymer composition. The repeated extrusion of the multistage gradient extrusion roller can enhance chemical reaction, improve surface texture, reduce deformation and dent marks, enable products to present a cavity structure, insulate sound and heat, and improve hardness to weight ratio; however, the technical method utilizes chemical reagent to produce foaming, the type of foaming cannot ensure the uniformity of each foaming core, the surface of the product is rough, the cost is high, and the light diffusion effect is poor.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a PP physical micro-foaming diffusion plate and a manufacturing method thereof.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a PP physical micro-foaming diffusion plate is prepared from the following raw materials in parts by weight: 100-120 parts of polypropylene, 1-3 parts of light diffusion agent master batch, 2-7 parts of nucleating agent, 20-30 parts of inorganic filler, 0.2-1.0 part of antioxidant and 1-2 parts of lubricant.
As a further preferable scheme of the invention, the light dispersing agent master batch is at least one of silicon dioxide, titanium dioxide, calcium carbonate and aluminum oxide;
The nucleating agent is boron nitride;
The antioxidant is at least one of hindered phenol antioxidants, phosphite antioxidants and hindered amine antioxidants;
the lubricant is at least one of polysiloxane, calcium stearate and zinc stearate.
As a further preferable embodiment of the present invention, the preparation method of the inorganic filler is as follows:
1) Respectively ultrasonically cleaning the porous nano cage material by using acetone, distilled water and ethanol for 30-50min, drying to obtain a pretreated porous nano cage material, dissolving antimony potassium tartrate in deionized water, magnetically stirring for 15-25min, adding polyvinylpyrrolidone, continuously stirring for 10-20min, adding thioacetamide into the formed mixed solution, and fully and uniformly stirring to obtain a reaction solution;
2) Adding the pretreated porous nano cage material into the reaction liquid, carrying out ultrasonic treatment for 10-20min, transferring to a reaction kettle, sealing, placing in an oven, heating at constant temperature for 24-28h, cooling to room temperature after the reaction is finished, centrifuging the product, repeatedly cleaning with deionized water, and drying to obtain the inorganic filler.
As a further preferable scheme of the invention, in the step 1), the dosage proportion of the antimony potassium tartrate, the deionized water, the polyvinylpyrrolidone and the thioacetamide is (0.4-0.7) mol: (30-60) mL: (0.2-0.5) g: (0.8-1.4) mol.
As a further preferable scheme of the invention, in the step 2), the dosage proportion of the pretreated porous nano cage material and the reaction solution is (3-7) g: (80-130) mL;
the power of the ultrasonic treatment is 150-200W;
The constant temperature heating temperature is 180-186 ℃.
As a further preferable scheme of the invention, the preparation method of the porous nano-cage material comprises the following steps:
1) Firstly weighing cobalt nitrate hexahydrate, then dissolving in methanol, fully stirring to obtain a solution A, then weighing 2-methylimidazole, dissolving in methanol, fully stirring to obtain a solution B, slowly pouring the solution B into an equal volume of the solution A, stirring at room temperature for 24-30h, centrifuging after stirring, repeatedly cleaning with methanol, and drying to obtain a metal organic framework material;
2) Adding a metal organic framework material into ethanol, fully stirring, adding cobalt nitrate hexahydrate, carrying out ultrasonic treatment for 15-20min, then refluxing in an oil bath pot at 90-95 ℃ for 3-5h, and centrifugally drying to obtain a precursor;
3) Spreading the precursor in a porcelain boat, spreading sodium hypophosphite monohydrate in another porcelain boat, placing two porcelain boats in a tube furnace, wherein sodium hypophosphite monohydrate is placed at the upstream of the air flow, placing the precursor at the downstream of the air flow, heating to 300-320 ℃ at a speed of 5-8 ℃/min under nitrogen atmosphere, preserving heat for 2-5h, and naturally cooling to room temperature to obtain the porous nano cage material.
As a further preferable mode of the invention, in the step 1), in the solution A, the dosage proportion of the cobalt nitrate hexahydrate and the methanol is (2.5-3.2) g: (200-280) mL;
In the solution B, the dosage ratio of the 2-methylimidazole to the methanol is (1.8-2.3) g: (200-280) mL.
As a further preferable scheme of the invention, in the step 2), the dosage proportion of the metal organic framework material, ethanol and cobalt nitrate hexahydrate is (0.3-0.8) g: (200-300) mL: (0.8-1.3) g;
The power of the ultrasonic treatment is 200-300W.
As a further preferred embodiment of the present invention, in step 3), the mass ratio of the precursor and sodium hypophosphite monohydrate is (0.2 to 0.6): (20-60).
A manufacturing method of a PP physical micro-foaming diffusion plate specifically comprises the following steps:
According to the parts by weight, polypropylene, light dispersing agent master batch, nucleating agent, inorganic filler, antioxidant and lubricant are put into a double-screw extruder, then supercritical nitrogen is evenly injected into a double-screw charging barrel at the flow rate of 40-70g/h, the extrusion temperature is 190-210 ℃, the extrusion section pressure is 7-9MPa, the static mixer partial pressure is 12-14MPa, the die pressure is 3-5MPa, and the required diffusion plate can be obtained after the materials are extruded and molded by the die.
Compared with the prior art, the invention has the beneficial effects that:
According to the invention, cobalt nitrate hexahydrate and 2-methylimidazole are used as raw materials to synthesize a metal organic framework material, and then the metal organic framework material is etched by adopting a cation exchange method, so that a porous nano cage material is obtained, the porous nano cage material basically maintains a rhombic dodecahedron framework, a large number of nano sheets exist on the surface, in the high-temperature treatment process, the internal solid structure is converted into a hollow structure, and the surface is an ultrathin nano sheet with a porous structure, so that the specific surface area is increased, and more active sites are provided; then cleaning the porous nano cage material to be used as a matrix material, taking antimony potassium tartrate and thioacetamide as an antimony source and a sulfur source respectively to form a reaction solution, adding the porous nano cage material into the reaction solution, performing hydrothermal reaction after full dispersion, depositing generated antimony sulfide nano particles to be attached to the surface of the porous nano cage material, and growing a plurality of netlike structures on the surface along with the progress of the hydrothermal reaction, wherein the deposited antimony sulfide nano particles gradually decrease along with the extension of the reaction time, the surface of the matrix material is covered by the antimony sulfide netlike structures with honeycomb structures, and the surface of the porous nano cage material is completely covered by the netlike structures along with complete disappearance of the antimony sulfide nano particles, so that an inorganic filler with a hollow structure is formed inside, and the outside is a supporting net structure formed by combination of nano sheets and the netlike structures; the inorganic filler is introduced into the diffusion plate, the injected nitrogen can enter the hollow area inside through the supporting net structure of the surface, so that the nitrogen is limited and fixed, cells are formed in the diffusion plate, when the inside of the inorganic filler and the supporting net of the surface are occupied by the nitrogen, the polymer material cannot permeate into the gaps of the inorganic filler, so that the cell structure cannot be damaged, and in the subsequent processing and forming process, the nitrogen in the cells gradually overflows, so that uniform cells can be formed in the diffusion plate.
According to the micro-foaming diffusion plate, the prepared inorganic filler is added into the polypropylene matrix, and foam holes which are uniformly distributed and basically consistent in size and aperture are formed in the diffusion plate in a supercritical nitrogen injection mode, so that the uniformity of foam cores is realized, and a better light diffusion effect can be achieved.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. 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 embodiment of the invention, the light diffusion agent master batch is silicon dioxide; the nucleating agent is boron nitride; the antioxidant is antioxidant 1010; the lubricant is calcium stearate.
Example 1
A PP physical micro-foaming diffusion plate is prepared from the following raw materials in parts by weight: 100 parts of polypropylene, 1 part of light diffusion agent master batch, 2 parts of nucleating agent, 20 parts of inorganic filler, 0.2 part of antioxidant and 1 part of lubricant;
The manufacturing method of the micro-foaming diffusion plate specifically comprises the following steps:
According to parts by weight, polypropylene, light dispersing agent master batch, nucleating agent, inorganic filler, antioxidant and lubricant are put into a double-screw extruder, then supercritical nitrogen is uniformly injected into a double-screw charging barrel at the flow of 40g/h, the extrusion temperature is 190 ℃, the extrusion section pressure is 7MPa, the static mixer partial pressure is 12MPa, the die pressure is 3MPa, and the required diffusion plate can be obtained after extruding the materials through a die.
The preparation method of the inorganic filler comprises the following steps:
1) Firstly weighing 2.5g of cobalt nitrate hexahydrate, then dissolving in 200mL of methanol, fully stirring to obtain a solution A, then weighing 1.8g of 2-methylimidazole, dissolving in 200mL of methanol, fully stirring to obtain a solution B, then slowly pouring the solution B into an equal volume of the solution A, stirring at room temperature for 24 hours, centrifuging after stirring, repeatedly cleaning with methanol, and drying to obtain a metal organic framework material;
2) Adding 0.3g of metal organic framework material into 200mL of ethanol, fully stirring, adding 0.8g of cobalt nitrate hexahydrate, performing ultrasonic treatment at 200W for 15min, refluxing in an oil bath at 90 ℃ for 3h, and centrifugally drying to obtain a precursor;
3) Spreading 0.2g of precursor in a porcelain boat, spreading 20g of sodium phosphite monohydrate in another porcelain boat, placing two porcelain boats in a tube furnace, wherein sodium phosphite monohydrate is placed at the upstream of the air flow, placing the precursor at the downstream of the air flow, heating to 300 ℃ at a speed of 5 ℃/min under nitrogen atmosphere, preserving heat for 2h, and naturally cooling to room temperature to obtain the porous nano cage material;
4) Respectively ultrasonically cleaning the porous nano cage material for 30min by using acetone, distilled water and ethanol in sequence, drying to obtain a pretreated porous nano cage material, dissolving 0.4mol of potassium antimony tartrate in 30mL of deionized water, magnetically stirring for 15min, adding 0.2g of polyvinylpyrrolidone, continuously stirring for 10min, then adding 0.8mol of thioacetamide into the formed mixed solution, and fully and uniformly stirring to obtain a reaction solution;
5) 3g of pretreated porous nano cage material is added into 80mL of reaction liquid, after being treated by 150W for 10min, the reaction liquid is transferred into a reaction kettle, and is sealed and then placed into a 180 ℃ oven for constant temperature heating for 24h, after the reaction is finished, the reaction liquid is cooled to room temperature, and after the product is centrifuged, the product is repeatedly washed by deionized water and dried, thus obtaining the inorganic filler.
Example 2
A PP physical micro-foaming diffusion plate is prepared from the following raw materials in parts by weight: 110 parts of polypropylene, 2 parts of light diffusion agent master batch, 5 parts of nucleating agent, 25 parts of inorganic filler, 0.6 part of antioxidant and 1.5 parts of lubricant;
The manufacturing method of the micro-foaming diffusion plate specifically comprises the following steps:
According to parts by weight, polypropylene, light dispersing agent master batch, nucleating agent, inorganic filler, antioxidant and lubricant are put into a double-screw extruder, then supercritical nitrogen is uniformly injected into a double-screw charging barrel at the flow rate of 60g/h, the extrusion temperature is 200 ℃, the extrusion section pressure is 8MPa, the static mixer partial pressure is 13MPa, the die pressure is 4MPa, and the required diffusion plate can be obtained after extruding the materials through a die.
The preparation method of the inorganic filler comprises the following steps:
1) Firstly weighing 3g of cobalt nitrate hexahydrate, then dissolving in 240mL of methanol, fully stirring to obtain a solution A, then weighing 2.1g of 2-methylimidazole, dissolving in 240mL of methanol, fully stirring to obtain a solution B, slowly pouring the solution B into an equal volume of the solution A, stirring at room temperature for 28 hours, centrifuging after stirring, repeatedly cleaning with methanol, and drying to obtain a metal organic framework material;
2) Adding 0.5g of metal organic framework material into 260mL of ethanol, fully stirring, adding 1.2g of cobalt nitrate hexahydrate, performing ultrasonic treatment at 250W for 18min, refluxing in an oil bath at 93 ℃ for 4h, and centrifugally drying to obtain a precursor;
3) Spreading 0.5g of precursor in a porcelain boat, spreading 50g of sodium phosphite monohydrate in another porcelain boat, placing two porcelain boats in a tube furnace, wherein sodium phosphite monohydrate is placed at the upstream of the air flow, placing the precursor at the downstream of the air flow, heating to 310 ℃ at a speed of 7 ℃/min under nitrogen atmosphere, preserving heat for 3 hours, and naturally cooling to room temperature to obtain the porous nano cage material;
4) Respectively ultrasonically cleaning the porous nano cage material by using acetone, distilled water and ethanol for 40min, drying to obtain a pretreated porous nano cage material, dissolving 0.5mol of potassium antimony tartrate in 50mL of deionized water, magnetically stirring for 20min, adding 0.3g of polyvinylpyrrolidone, continuously stirring for 15min, then adding 1.2mol of thioacetamide into the formed mixed solution, and fully and uniformly stirring to obtain a reaction solution;
5) Adding 5g of pretreated porous nano cage material into 110mL of reaction liquid, carrying out 180W ultrasonic treatment for 15min, transferring into a reaction kettle, sealing, placing into a 183 ℃ oven, heating at constant temperature for 26h, cooling to room temperature after the reaction is finished, centrifuging the product, repeatedly cleaning with deionized water, and drying to obtain the inorganic filler.
Example 3
A PP physical micro-foaming diffusion plate is prepared from the following raw materials in parts by weight: 120 parts of polypropylene, 3 parts of light diffusion agent master batch, 7 parts of nucleating agent, 30 parts of inorganic filler, 1 part of antioxidant and 2 parts of lubricant;
The manufacturing method of the micro-foaming diffusion plate specifically comprises the following steps:
According to parts by weight, polypropylene, light dispersing agent master batch, nucleating agent, inorganic filler, antioxidant and lubricant are put into a double-screw extruder, then supercritical nitrogen is uniformly injected into a double-screw charging barrel at the flow rate of 70g/h, the extrusion temperature is 210 ℃, the extrusion section pressure is 9MPa, the static mixer partial pressure is 14MPa, the die pressure is 5MPa, and the required diffusion plate can be obtained after extruding the materials through a die.
The preparation method of the inorganic filler comprises the following steps:
1) Firstly weighing 3.2g of cobalt nitrate hexahydrate, then dissolving in 280mL of methanol, fully stirring to obtain a solution A, then weighing 2.3g of 2-methylimidazole, dissolving in 280mL of methanol, fully stirring to obtain a solution B, then slowly pouring the solution B into an equal volume of the solution A, stirring at room temperature for 30 hours, centrifuging after stirring, repeatedly cleaning with methanol, and drying to obtain a metal organic framework material;
2) Adding 0.8g of metal organic framework material into 300mL of ethanol, fully stirring, adding 1.3g of cobalt nitrate hexahydrate, performing ultrasonic treatment at 300W for 20min, refluxing in an oil bath at 95 ℃ for 5h, and centrifugally drying to obtain a precursor;
3) Spreading 0.6g of precursor in a porcelain boat, spreading 60g of sodium phosphite monohydrate in another porcelain boat, placing two porcelain boats in a tube furnace, wherein sodium phosphite monohydrate is placed at the upstream of the air flow, placing the precursor at the downstream of the air flow, heating to 320 ℃ at a speed of 8 ℃/min under nitrogen atmosphere, preserving heat for 5h, and naturally cooling to room temperature to obtain the porous nano cage material;
4) Respectively ultrasonically cleaning the porous nano cage material by using acetone, distilled water and ethanol for 50min, drying to obtain a pretreated porous nano cage material, dissolving 0.7mol of potassium antimony tartrate in 60mL of deionized water, magnetically stirring for 25min, adding 0.5g of polyvinylpyrrolidone, continuously stirring for 20min, then adding 1.4mol of thioacetamide into the formed mixed solution, and fully and uniformly stirring to obtain a reaction solution;
5) Adding 7g of pretreated porous nano cage material into 130mL of reaction liquid, carrying out 200W ultrasonic treatment for 20min, transferring into a reaction kettle, sealing, placing into a 186 ℃ oven, heating at constant temperature for 28h, cooling to room temperature after the reaction is finished, centrifuging the product, repeatedly cleaning with deionized water, and drying to obtain the inorganic filler.
Comparative example 1: this comparative example is substantially the same as example 1 except that no inorganic filler is contained.
Comparative example 2: this comparative example is substantially the same as example 1, except that step 1) is omitted in the preparation of the inorganic filler.
Comparative example 3: this comparative example is substantially the same as example 1, except that step 2) is omitted in the preparation of the inorganic filler.
Comparative example 4: this comparative example is essentially the same as example 1, except that steps 1) -3 are omitted in the preparation of the inorganic filler.
Comparative example 5: this comparative example is essentially the same as example 1, except that steps 4) to 5) are omitted in the preparation of the inorganic filler.
Test experiment:
Samples of the micro-foaming diffusion plates were prepared by the methods disclosed in examples 1 to 3 and comparative examples 1 to 5, respectively, and then subjected to light transmittance test with reference to GB/T241012008, and the results are shown in Table 1.
TABLE 1
As is clear from Table 1, the micro-foam diffusion plate of the present invention has excellent light diffusion effect, and the light transmittance is not less than 90%.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiment does not describe all details in detail nor limit the invention to the specific embodiments described. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (10)
1. The PP physical micro-foaming diffusion plate is characterized by being prepared from the following raw materials in parts by weight: 100-120 parts of polypropylene, 1-3 parts of light diffusion agent master batch, 2-7 parts of nucleating agent, 20-30 parts of inorganic filler, 0.2-1.0 part of antioxidant and 1-2 parts of lubricant.
2. The PP physical-micro-foam diffusion plate of claim 1, wherein the light diffusing agent master batch is at least one of silica, titanium dioxide, calcium carbonate, and alumina;
The nucleating agent is boron nitride;
The antioxidant is at least one of hindered phenol antioxidants, phosphite antioxidants and hindered amine antioxidants;
the lubricant is at least one of polysiloxane, calcium stearate and zinc stearate.
3. The PP physical-micro-foaming diffusion plate according to claim 1, wherein the inorganic filler is prepared by the following method:
1) Respectively ultrasonically cleaning the porous nano cage material by using acetone, distilled water and ethanol for 30-50min, drying to obtain a pretreated porous nano cage material, dissolving antimony potassium tartrate in deionized water, magnetically stirring for 15-25min, adding polyvinylpyrrolidone, continuously stirring for 10-20min, adding thioacetamide into the formed mixed solution, and fully and uniformly stirring to obtain a reaction solution;
2) Adding the pretreated porous nano cage material into the reaction liquid, carrying out ultrasonic treatment for 10-20min, transferring to a reaction kettle, sealing, placing in an oven, heating at constant temperature for 24-28h, cooling to room temperature after the reaction is finished, centrifuging the product, repeatedly cleaning with deionized water, and drying to obtain the inorganic filler.
4. The PP physical micro-foam diffusion plate according to claim 3, wherein in step 1), the amount ratio of antimony potassium tartrate, deionized water, polyvinylpyrrolidone, thioacetamide is (0.4-0.7) mol: (30-60) mL: (0.2-0.5) g: (0.8-1.4) mol.
5. The PP physical micro-foaming diffusion plate according to claim 3, wherein in the step 2), the ratio of the amount of the pretreated porous nanocage material to the amount of the reaction solution is (3-7) g: (80-130) mL;
the power of the ultrasonic treatment is 150-200W;
The constant temperature heating temperature is 180-186 ℃.
6. The PP physical micro-foam diffusion plate of claim 3, wherein the porous nanocage material is prepared by the following method:
1) Firstly weighing cobalt nitrate hexahydrate, then dissolving in methanol, fully stirring to obtain a solution A, then weighing 2-methylimidazole, dissolving in methanol, fully stirring to obtain a solution B, slowly pouring the solution B into an equal volume of the solution A, stirring at room temperature for 24-30h, centrifuging after stirring, repeatedly cleaning with methanol, and drying to obtain a metal organic framework material;
2) Adding a metal organic framework material into ethanol, fully stirring, adding cobalt nitrate hexahydrate, carrying out ultrasonic treatment for 15-20min, then refluxing in an oil bath pot at 90-95 ℃ for 3-5h, and centrifugally drying to obtain a precursor;
3) Spreading the precursor in a porcelain boat, spreading sodium hypophosphite monohydrate in another porcelain boat, placing two porcelain boats in a tube furnace, wherein sodium hypophosphite monohydrate is placed at the upstream of the air flow, placing the precursor at the downstream of the air flow, heating to 300-320 ℃ at a speed of 5-8 ℃/min under nitrogen atmosphere, preserving heat for 2-5h, and naturally cooling to room temperature to obtain the porous nano cage material.
7. The PP physical-micro-foam diffusion plate according to claim 6, wherein in step 1), the amount ratio of cobalt nitrate hexahydrate to methanol in the solution a is (2.5-3.2) g: (200-280) mL;
In the solution B, the dosage ratio of the 2-methylimidazole to the methanol is (1.8-2.3) g: (200-280) mL.
8. The PP physical-micro-foam diffusion plate according to claim 6, wherein in step 2), the metal-organic framework material, ethanol, and cobalt nitrate hexahydrate are used in a ratio of (0.3-0.8) g: (200-300) mL: (0.8-1.3) g;
The power of the ultrasonic treatment is 200-300W.
9. The PP physical-micro-foam diffusion plate of claim 6, wherein in step 3), the mass ratio of the precursor and sodium hypophosphite monohydrate is (0.2-0.6): (20-60).
10. The method for manufacturing a PP physical micro-foaming diffusion plate according to any one of claims 1 to 9, comprising the steps of:
According to the parts by weight, polypropylene, light dispersing agent master batch, nucleating agent, inorganic filler, antioxidant and lubricant are put into a double-screw extruder, then supercritical nitrogen is evenly injected into a double-screw charging barrel at the flow rate of 40-70g/h, the extrusion temperature is 190-210 ℃, the extrusion section pressure is 7-9MPa, the static mixer partial pressure is 12-14MPa, the die pressure is 3-5MPa, and the required diffusion plate can be obtained after the materials are extruded and molded by the die.
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