CN108976639A - The production method of nano-high molecule bamboo and woods fiber integrated wall plate - Google Patents
The production method of nano-high molecule bamboo and woods fiber integrated wall plate Download PDFInfo
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- CN108976639A CN108976639A CN201710420759.9A CN201710420759A CN108976639A CN 108976639 A CN108976639 A CN 108976639A CN 201710420759 A CN201710420759 A CN 201710420759A CN 108976639 A CN108976639 A CN 108976639A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D99/00—Subject matter not provided for in other groups of this subclass
- B29D99/001—Producing wall or panel-like structures, e.g. for hulls, fuselages, or buildings
-
- 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
- C08J9/06—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 chemical blowing agent
- C08J9/10—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 chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F13/00—Coverings or linings, e.g. for walls or ceilings
- E04F13/07—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor
- E04F13/08—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements
- E04F13/0875—Coverings or linings, e.g. for walls or ceilings composed of covering or lining elements; Sub-structures therefor; Fastening means therefor composed of a plurality of similar covering or lining elements having a basic insulating layer and at least one covering layer
-
- 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
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
-
- 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
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
-
- 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
- C08J2497/00—Characterised by the use of lignin-containing materials
- C08J2497/02—Lignocellulosic material, e.g. wood, straw or bagasse
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Architecture (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
Abstract
The present invention relates to a kind of production method of nano-high molecule bamboo and woods fiber integrated wall plate, the raw materials used integrated wall plate includes Corvic, Paris white, bamboo powder, stearic acid, foaming agent, foaming control agent, calcium zinc stabilizer;Production stage is: raw material being uniformly mixed, extrusion shaping machine is transferred to, forms the molding semi product that there is the cavity of multicell to construct;Traction stretching is carried out, shaper is covered and vacuumize being extruded to shape, forms wallboard substrate;High temperature overlay film is carried out on wallboard substrate, is then cut by setting specification, nano-high molecule bamboo and woods fiber integrated wall plate is made.
Description
Technical field
The present invention relates to a kind of production methods of nano-high molecule bamboo and woods fiber integrated wall plate, by heatmeltable resin, modification
By foam extrusion process, traction setting process, coating technique, be made has the raw materials such as filler material, functional additive, adhesive
The wall board material of simulated effect, the decoration for inner wall of building.
Background technique
Chinese patent 201611069029.0 discloses a kind of combined wall board, raw material roll bending is put into embossing unit, through locating
Raw material plate after reason is put into cold roll forming unit, after handling in cold roll forming unit, sets on obtained raw material roll bending upper berth poly-
Ammoniacum layer sets up defences fire bed on polyurethane layer upper berth, combined wall board is made.This combined wall board has can be with Fast Installation, heat preservation
Heat-insulated, flat noise reduction, light wear-resisting feature.
But the thickness of this kind of combined wall board can reach 50 millimeters, be only applicable to exterior walls of buildings, be not suitable as building
The decoration of object inner wall surface.Accordingly, it is desirable to provide a kind of production method of nano-high molecule bamboo and woods fiber integrated wall plate, uses the party
Legal system takes wall board material, the decoration for inner wall of building face.
Summary of the invention
The purpose of the present invention is to provide a kind of production method of nano-high molecule bamboo and woods fiber integrated wall plate, the integrated walls
Raw materials used plate includes Corvic, Paris white, bamboo powder, stearic acid, foaming agent, foaming control agent, stabilizer;It will
Raw material is uniformly mixed, and is transferred to extrusion shaping machine, carries out traction stretching, is covered shaper and vacuumize being extruded to shape,
Form wallboard substrate;High temperature overlay film is carried out on wallboard substrate;This integrated wall plate have can with Fast Installation, insulation,
Sound-deadening and noise-reducing, light wear-resisting feature, the decoration for inner wall of building face.
The purpose of the present invention is what is realized by following technical proposals: a kind of life of nano-high molecule bamboo and woods fiber integrated wall plate
Production method, the raw materials used parts by weight component of the wallboard include Corvic 10-15, Paris white 21-23, bamboo powder
0.5-0.6, stearic acid 5-7, foaming agent 0.7-0.8, foaming control agent 0.6-0.7, calcium-zinc composite stabilizing agent 49-52;The life
Producing step is:
A, the raw material is put into the mixed machine high-speed stirred of heat to be uniformly mixed, is warming up to 110 DEG C of -115 DEG C of holdings 5 minutes, so
Raw material is transferred to cold mixer stirring cooling again afterwards, 55 DEG C -58 DEG C of cooling temperature, is formed and mixes material;
B, mixing material is transferred to extrusion shaping machine, the mixing material enters merging core after stepped heating, enters back into
Mold and hot briquetting, being formed, there is the cavity of multicell to construct, and be capable of forming the molding semi product of cross-ventilation circulation;
C, the molding semi product is subjected to traction stretching by dragger in conventionally speed in the production line, covered simultaneously
Shaper vacuumize being extruded to shape, and forms wallboard substrate;
D, substrate glue and PVC film are subjected to high temperature overlay film, are then cut by setting specification, nanometer is made
Macromolecule bamboo and woods fiber integrated wall plate.
Compared with the prior art the present invention has the advantages that
1, the present invention realizes the modification of inorganic powder material, but also more by some prices by the modification to filler
Add cheap biological material to be added in product, improves the multinomial performance index of wallboard product well.
2, the weatherability of wall board material produced by the invention greatly improves, wherein cold-resistant thermal circulation performance improves 31%.
3, the filler used in the present invention has the characteristics that purity is high, environmental protection, lubricity are good, can not only raw material be assisted to send out
Bubble also has modifying function to raw material, improves the coupling between biomass and polymer, enhances wallboard strength, and plays steady
Determine agent and dispersing agent function.
4, wallboard product produced by the invention, physical mechanical property can be compared with hardwood, and can be made by overlay film has
The dalle of simulated effect.
Specific embodiment
Embodiment one:
In the production method of nano-high molecule bamboo and woods fiber integrated wall plate of the invention, raw materials used parts by weight component packet
Include Corvic 10-15, Paris white 21-23, bamboo powder 0.5-0.6, stearic acid 5-7, foaming agent 0.7-0.8, foaming
Regulator 0.6-0.7, calcium-zinc composite stabilizing agent 49-52;The production stage is:
A, the raw material is put into the mixed machine high-speed stirred of heat to be uniformly mixed, is warming up to 110 DEG C of -115 DEG C of holdings 5 minutes, most
Good temperature is 115 DEG C, and raw material is then transferred to cold mixer stirring cooling again, and cooling temperature is 55 DEG C -58 DEG C, is formed and mixes material,
Best cooling temperature is 58 DEG C;
B, mixing material is transferred to extrusion shaping machine, the mixing material enters merging core after stepped heating, enters back into
Mold and hot briquetting, being formed, there is the cavity of multicell to construct, and be capable of forming the molding semi product of cross-ventilation circulation;The sky
Chamber construction refers to the rectangle duct construction of a plurality of side-by-side parallel.
C, the molding semi product is subjected to traction stretching by dragger in conventionally speed in the production line, covered simultaneously
Shaper vacuumize being extruded to shape, and forms wallboard substrate;
D, substrate glue and PVC film are subjected to high temperature overlay film, are then cut by setting specification, nanometer is made
Macromolecule bamboo and woods fiber integrated wall plate plate, the integrated wall plate plate with a thickness of 6-10mm, the optimum thickness of plate be 9 milli
Rice.
In the present invention, the parts by weight component of the raw material can also be Corvic 10, Paris white 22.5, bamboo and wood
Powder 0.5, stearic acid 5, foaming agent 0.8, foaming control agent 0.65, calcium-zinc composite stabilizing agent 50.6;50% is in the bamboo powder
Nanoscale is carbonized bamboo fibre powder, and 5% is nanoscale Paris white in the Paris white.In the present invention, the polychlorostyrene second
Olefine resin is that emulsion method polyvinyl chloride resin is mixed with suspension pvc resin 1: 1, and the foaming agent is ADC (azodicarbonamide), institute
Stating calcium-zinc composite stabilizing agent is one of CH400, CH401, CH402 Ca-Zn composite heat stabilizer.Foaming control agent is DLP-
100.Paris white is 60-100 mesh powder.
Product strength made of the present invention is high, the service life is long, due to the stability of microcellular structure, ensure that the mechanical property of material
Can, fretting map without residual stress, the good stability of the dimension of product is pressure-resistant, and impact property is remarkably reinforced, and overcomes common PVC system
The low defect of product cracky, strength of wood, service life was up to 30 years or more.
Product made of the present invention has the excellent physical and chemical performance such as corrosion-resistant, moisture-proof, fire-retardant, heat-insulated, insulation, and
And the secondary operation such as it is easy to bond, saw, digging, boring, cutting.
In addition, using non-toxic formulation and on-liquid auxiliary agent in production process of the present invention, the substantially non-volatile object of product belongs to
Environmental type material.
In the present embodiment, the mixed machine high-speed stirred mixing of heat refers to that (model is 800/ using commercially available high-speed mixer
2600) processing carried out.Extrusion shaping machine is double screw extruder (model is SJZ65/135), draws stretcher, stock mould
Have equipment, vacuumize the equipment that is extruded to shape, is that equipment is sold in market, is not described in detail.
Claims (3)
1. a kind of production method of nano-high molecule bamboo and woods fiber integrated wall plate, it is characterised in that: the wallboard is raw materials used
Parts by weight component includes Corvic 10-15, Paris white 21-23, bamboo powder 0.5-0.6, stearic acid 5-7, foaming agent
0.7-0.8, foaming control agent 0.6-0.7, calcium-zinc composite stabilizing agent 49-52;The production stage is:
A, the raw material is put into the mixed machine high-speed stirred of heat to be uniformly mixed, is warming up to 110 DEG C of -115 DEG C of holdings 5 minutes, then again
Raw material is transferred to cold mixer stirring cooling, 55 DEG C -58 DEG C of cooling temperature, is formed and mixes material;
B, mixing material is transferred to extrusion shaping machine, the mixing material enters merging core after stepped heating, enters back into mold
And hot briquetting, being formed, there is the cavity of multicell to construct, and be capable of forming the molding semi product of cross-ventilation circulation;
C, the molding semi product is subjected to traction stretching by dragger in conventionally speed in the production line, while covers sizing
Mold vacuumize being extruded to shape, and forms wallboard substrate;
D, substrate glue and PVC film are subjected to high temperature overlay film, are then cut by setting specification, nanometer high score is made
Sub- bamboo and woods fiber integrated wall plate.
2. the production method of integrated wall plate according to claim 1, it is characterised in that: the parts by weight component packet of the raw material
Include Corvic 10, Paris white 22.5, bamboo powder 0.5, stearic acid 5, foaming agent 0.8, foaming control agent 0.65, calcium zinc
Compound stabilizer 50.6;50% is nanoscale carbonization bamboo fibre powder in the bamboo powder, and 5% is nanometer in the Paris white
The Paris white of grade.
3. the production method of integrated wall plate according to claim 1, it is characterised in that: the Corvic is lotion
Method polyvinyl chloride resin is mixed with suspension pvc resin 1: 1, and the foaming agent is ADC (azodicarbonamide), and the Ca Zn composite is steady
Determining agent is one of CH400, CH401, CH402 Ca-Zn composite heat stabilizer.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109825103A (en) * | 2019-01-21 | 2019-05-31 | 泸州锦兰科技有限公司 | A kind of finishing bamboo fibre plate and preparation method thereof |
CN109971097A (en) * | 2019-04-25 | 2019-07-05 | 湖南恒信新型建材有限公司 | A kind of environmentally protective bamboo and woods fiber circuit board and its manufacturing method |
CN110271159A (en) * | 2019-05-27 | 2019-09-24 | 福建祥龙塑胶有限公司 | A kind of manufacturing method of wallboard |
CN110283399A (en) * | 2019-05-06 | 2019-09-27 | 浙江中财管道科技股份有限公司 | A kind of bamboo and woods fiber wallboard and preparation method thereof |
CN110760142A (en) * | 2019-11-11 | 2020-02-07 | 湘木豪廷新材料有限公司 | High-strength bamboo-wood fiber integrated wallboard and processing method thereof |
CN112812471A (en) * | 2021-01-24 | 2021-05-18 | 湖北欧宅新材料科技有限公司 | Environment-friendly wear-resistant bamboo-wood fiber wallboard and preparation method thereof |
CN114013002A (en) * | 2021-11-04 | 2022-02-08 | 浙江欧舍家居新材股份有限公司 | Production process of micro-foaming PVC (polyvinyl chloride) plate |
CN114276629A (en) * | 2021-11-19 | 2022-04-05 | 东台市豪威节能科技有限公司 | Preparation method of bamboo-wood fiber heat-insulation composite decorative plate |
-
2017
- 2017-06-01 CN CN201710420759.9A patent/CN108976639A/en active Pending
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109825103A (en) * | 2019-01-21 | 2019-05-31 | 泸州锦兰科技有限公司 | A kind of finishing bamboo fibre plate and preparation method thereof |
CN109971097A (en) * | 2019-04-25 | 2019-07-05 | 湖南恒信新型建材有限公司 | A kind of environmentally protective bamboo and woods fiber circuit board and its manufacturing method |
CN109971097B (en) * | 2019-04-25 | 2021-02-02 | 湖南恒信新型建材有限公司 | Green environment-friendly bamboo-wood fiber integrated board and manufacturing method thereof |
CN110283399A (en) * | 2019-05-06 | 2019-09-27 | 浙江中财管道科技股份有限公司 | A kind of bamboo and woods fiber wallboard and preparation method thereof |
CN110283399B (en) * | 2019-05-06 | 2022-04-26 | 浙江中财管道科技股份有限公司 | Bamboo-wood fiber wallboard and preparation method thereof |
CN110271159A (en) * | 2019-05-27 | 2019-09-24 | 福建祥龙塑胶有限公司 | A kind of manufacturing method of wallboard |
CN110760142A (en) * | 2019-11-11 | 2020-02-07 | 湘木豪廷新材料有限公司 | High-strength bamboo-wood fiber integrated wallboard and processing method thereof |
CN112812471A (en) * | 2021-01-24 | 2021-05-18 | 湖北欧宅新材料科技有限公司 | Environment-friendly wear-resistant bamboo-wood fiber wallboard and preparation method thereof |
CN114013002A (en) * | 2021-11-04 | 2022-02-08 | 浙江欧舍家居新材股份有限公司 | Production process of micro-foaming PVC (polyvinyl chloride) plate |
CN114276629A (en) * | 2021-11-19 | 2022-04-05 | 东台市豪威节能科技有限公司 | Preparation method of bamboo-wood fiber heat-insulation composite decorative plate |
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Application publication date: 20181211 |
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WD01 | Invention patent application deemed withdrawn after publication |