CN110498999B - Nitrogen-oxygen separation carrier phenolic foam product and preparation method thereof - Google Patents
Nitrogen-oxygen separation carrier phenolic foam product and preparation method thereof Download PDFInfo
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- CN110498999B CN110498999B CN201910824758.XA CN201910824758A CN110498999B CN 110498999 B CN110498999 B CN 110498999B CN 201910824758 A CN201910824758 A CN 201910824758A CN 110498999 B CN110498999 B CN 110498999B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/047—Pressure swing adsorption
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- 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
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
-
- 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
- C08J9/0014—Use of organic additives
- C08J9/0033—Use of organic additives containing sulfur
-
- 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
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- 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
- C08J9/14—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 organic
- C08J9/141—Hydrocarbons
-
- 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
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
-
- 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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/329—Phosphorus containing acids
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
Abstract
The invention provides a nitrogen-oxygen separation carrier phenolic foam product and a preparation method thereof, wherein the nitrogen-oxygen separation carrier phenolic foam product comprises the following components in parts by mass: 100 parts of high-performance phenolic resin, 20-35 parts of curing agent, 5-15 parts of foaming agent, 5-15 parts of wetting agent, 3-6 parts of cell opener, 2.5-3.5 parts of ethanol, 1-1.5 parts of butanol and 0.1-0.5 part of sodium butoxide; wherein the curing agent is a mixture of deionized water, phosphoric acid and p-toluenesulfonic acid, and the ratio of deionized water: phosphoric acid: the p-toluenesulfonic acid ratio was 37:37: 100. Compared with the products on the market at present, the phenolic foam product with the nitrogen-oxygen separation carrier prepared by the invention has the advantages of lower ash content, high aperture ratio, strong water absorption, and favorable preparation of the nitrogen-oxygen separation carrier by volatile components, and can improve the nitrogen preparation concentration and the nitrogen preparation rate.
Description
Technical Field
The invention relates to the field of nitrogen-oxygen separation carrier materials, in particular to a nitrogen-oxygen separation carrier phenolic foam product and a preparation method thereof.
Background
There are currently three main processes for separating oxygen and nitrogen from air, including: membrane separation technology, Pressure Swing Adsorption (PSA) technology, and deep freezing technology. The pressure swing adsorption technology utilizes a molecular sieve as an adsorbent, and works through the characteristic of selective adsorption of the adsorbent to gas.
It is known that to obtain a nitrogen-oxygen separation carrier (i.e. a nitrogen-producing carbon molecular sieve) with excellent performance, the basic raw material needs to have the following properties: the lower the ash content, the better (about 4.5% of the ash content of the base material used in the current market), the volatile matter needs to be in the range of 44% -48%, the moisture content should be lower than 20%, and the mass water absorption of the base material should be controlled to be 5-40 times.
The nitrogen-oxygen separation carrier prepared by the prior art generally adopts flower mud as a basic raw material, the raw material belongs to open-cell foam, generally has high ash content and volatile components, and has imperfect water and water absorption performance, the nitrogen-oxygen separation carrier produced by using the flower mud as the basic raw material has low yield, and meanwhile, the nitrogen production rate by using the carrier is low, and the nitrogen production concentration is low.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides a nitrogen-oxygen separation carrier phenolic foam product which comprises the following components in parts by mass: 100 parts of high-performance phenolic resin, 20-35 parts of curing agent, 5-15 parts of foaming agent, 5-15 parts of wetting agent, 3-6 parts of cell opener, 2.5-3.5 parts of ethanol, 1-1.5 parts of butanol and 0.1-0.5 part of sodium butoxide;
wherein, the curing agent is a mixture of deionized water, phosphoric acid and p-toluenesulfonic acid, and the mass ratio of the deionized water: phosphoric acid: the p-toluenesulfonic acid ratio was 37:37: 100.
Further, the viscosity of the high-performance phenolic resin is 5000-10000cp at 25 ℃, the free phenol is less than or equal to 2.5%, the free aldehyde is less than or equal to 0.5%, and the solid content is more than or equal to 82%.
Further, the purity of the p-toluenesulfonic acid is more than or equal to 99.9%.
Further, the foaming agent is n-pentane, n-hexane or isopentane.
Further, the wetting agent is a surfactant with HLB value of 7-9.
Further, the cell opener is AES, sodium dodecyl benzene sulfonate, liquid detergent and the like.
The invention also provides a preparation method of the nitrogen-oxygen separation carrier phenolic foam product, which comprises the following steps:
step one, putting high-performance phenolic resin, a foaming agent, a wetting agent, a pore-opening agent, ethanol, butanol and sodium butoxide into a stirring tank according to a proportion, stirring, and uniformly mixing for later use;
step two, conveying the mixture to a pouring head through a conveying pipe, quickly and uniformly stirring the mixture and a curing agent in the other conveying pipe, pouring the mixture into a heated laminating machine, and laminating;
and step three, sending the material to a drying room, and carrying out rising, curing, forming and demoulding to obtain the nitrogen-oxygen separation carrier phenolic foam product.
Furthermore, recyclable plastic films are paved on the upper surface and the lower surface of the laminating machine.
Furthermore, the temperature of the drying room is 75-85 ℃, the length of the production line of the drying device is 18 meters, and the speed of the chain plate is 1.2-1.5 m/s.
The invention provides a nitrogen-oxygen separation carrier phenolic foam product, wherein the curing agent in the components is a curing agent generally adopted in the preparation process of phenolic foam, namely a mixture of deionized water, phosphoric acid and p-toluenesulfonic acid, and the weight ratio of the deionized water: phosphoric acid: the p-toluenesulfonic acid ratio was 37:37: 100. In order to effectively reduce the ash content of the phenolic foam product, the components of the invention are added with ethanol, butanol and sodium butoxide, and the ash content of the phenolic foam product is obviously reduced by effectively reacting the three additives with other components in the components.
Compared with the basic raw materials of the nitrogen-oxygen separation carrier on the market at present, the prepared nitrogen-oxygen separation carrier phenolic foam product has the advantages of lower ash content, high aperture ratio, strong water absorbability and more favorable volatile components for preparing the nitrogen-oxygen separation carrier, and can improve the nitrogen preparation concentration and the nitrogen preparation rate. Has positive popularization significance for the industry.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
It should be noted that the reagents or apparatuses used in the examples are not indicated by the manufacturer, but those not indicated by the specific techniques or conditions described in the literature in the art or by the specifications of the products are all conventional products commercially available.
The reagents of the examples and comparative examples of the invention are illustrated below:
high-performance phenolic resin: 2.7 percent of free phenol, 0.4 percent of free aldehyde, 85 percent of solid content and 6000cp of viscosity at 25 ℃.
Curing agent: (deionized water: phosphoric acid: p-toluenesulfonic acid) ratio was (37:37: 100).
Foaming agent: n-pentane.
Wetting agent: a span.
A pore forming agent: sodium dodecyl benzene sulfonate.
The component formulas (in parts by mass) of examples 1 to 3 provided by the invention are shown in table 1:
TABLE 1
The phenolic foam articles of examples 1-3 were prepared as follows:
step one, putting high-performance phenolic resin, a foaming agent, a wetting agent, a pore-opening agent, ethanol, butanol and sodium butoxide into a stirring tank according to the proportion of the components, stirring and uniformly mixing for later use;
step two, conveying the mixture to a pouring head through a conveying pipe, quickly and uniformly stirring the mixture and a curing agent in the other conveying pipe, pouring the mixture into a heated laminating machine, and pressing the mixture, wherein the size of a mold is 300 x 25 mm;
step three, the materials are sent to a drying room, the temperature of the drying room is controlled to be about 80 ℃, the materials are placed in the drying room for rising, and after 15min, the materials are cured, molded and subjected to demoulding to obtain a nitrogen-oxygen separation carrier phenolic foam product; the length of the production line is 18m, and the speed of the chain plate is 1.2-1.5 m/s; and (5) demoulding quickly when the mould is hot after demoulding.
The formula (in parts by mass) of the components of comparative examples 1 to 7 provided by the present invention is shown in table 2:
TABLE 2
Note: means the formulation is without the addition of this component.
The phenolic foam articles of comparative examples 1-7 were prepared as follows:
step one, putting high-performance phenolic resin, a foaming agent, a wetting agent, a pore-forming agent, ethanol, butanol and sodium butoxide into a stirring tank according to the component proportion, and uniformly mixing for later use; wherein, the comparative example 1 does not add ethanol, butanol, sodium butoxide; comparative example 2 no butanol, sodium butoxide were added; comparative example 3 no ethanol, sodium butoxide were added; comparative example 4 no ethanol, butanol were added; comparative example 5 no sodium butoxide was added; comparative example 6 no butanol was added; comparative example 7 no ethanol was added;
step two, conveying the mixture to a pouring head through a conveying pipe, quickly and uniformly stirring the mixture and a curing agent in the other conveying pipe, pouring the mixture into a heated laminating machine, and pressing the mixture, wherein the size of a mold is 300 x 25 mm;
step three, the materials are sent to a drying room, the temperature of the drying room is controlled to be about 80 ℃, the materials are placed in the drying room for rising, and after 15min, the materials are cured, molded and subjected to demoulding to obtain a nitrogen-oxygen separation carrier phenolic foam product; the length of the production line is 18m, and the speed of the chain plate is 1.2-1.5 m/s; and (4) demoulding quickly when the mould is hot after demoulding.
The present invention performed relevant physical and chemical tests on the phenolic foams prepared in examples 1-3 and comparative examples 1-7, and the test results are shown in Table 3:
TABLE 3
As can be seen from table 1, the ash content of the phenolic foam obtained in example 1 is 0.35%, the ash content of the phenolic foam obtained in example 2 is 0.4%, and the ash content of the phenolic foam obtained in example 3 is 0.32%, so that the ash content of the base material of the nitrogen-oxygen separation carrier prepared by using the phenolic foam product provided by the present invention is much lower than that of the base material of the nitrogen-oxygen separation carrier on the market. The nitrogen-oxygen separation carrier prepared by the phenolic foam product provided by the invention can improve the nitrogen preparation concentration and the nitrogen preparation rate.
As can be seen from Table 1, the composition of comparative example 1 lacks ethanol, butanol and sodium butoxide compared to the examples, and the ash content of the phenolic foam product produced is 3.8%. The composition of comparative example 2, lacking butanol, sodium butoxide compared to the examples, produced a phenolic foam product with an ash of 3.2%. The composition of comparative example 3 lacks ethanol, sodium butoxide compared to the examples, and the phenolic foam product produced has an ash content of 3.1%. The composition of comparative example 4 lacks ethanol, butanol compared to the examples, and the ash content of the phenolic foam product produced is 2.9%. The composition of comparative example 5, lacking sodium butoxide compared to the examples, produced phenolic foam products with ash of 2.8%. The composition of comparative example 6, lacking butanol as compared to the examples, produced phenolic foam products with ash of 2.7%. The composition of comparative example 1 lacks ethanol compared to the examples and produces phenolic foam products with an ash of 3.5%. Therefore, the co-existence of the ethanol, the butanol and the sodium butoxide in the components of the invention can generate the synergistic effect with other components in the components, thereby effectively reducing the ash content of the phenolic foam product. Any one of the three components is omitted, the synergistic effect with other components in the components disappears, and the ash content of the phenolic foam product cannot be effectively reduced.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. A nitrogen-oxygen separation carrier phenolic foam product is characterized in that: the composition comprises the following components in parts by mass: 100 parts of high-performance phenolic resin, 20-35 parts of curing agent, 5-15 parts of foaming agent, 5-15 parts of wetting agent, 3-6 parts of cell opener, 2.5-3.5 parts of ethanol, 1-1.5 parts of butanol and 0.1-0.5 part of sodium butoxide;
wherein, the curing agent is a mixture of deionized water, phosphoric acid and p-toluenesulfonic acid, and the mass ratio of the deionized water: phosphoric acid: the p-toluenesulfonic acid ratio was 37:37: 100.
2. The nitrogen oxygen separation carrier phenolic foam article of claim 1, wherein: the high-performance phenolic resin has the viscosity of 10000cP of 5000-plus at 25 ℃, the content of free phenol is less than or equal to 2.5 percent, the content of free aldehyde is less than or equal to 0.5 percent, and the solid content is more than or equal to 82 percent.
3. The nitrogen oxygen separation carrier phenolic foam article of claim 1, wherein: the purity of the p-toluenesulfonic acid is more than or equal to 99.9 percent.
4. The nitrogen oxygen separation carrier phenolic foam article of claim 1, wherein: the foaming agent is n-pentane, n-hexane or isopentane.
5. The nitrogen oxygen separation carrier phenolic foam article of claim 1, wherein: the wetting agent is a surfactant with an HLB value of 7-9.
6. The nitrogen oxygen separation carrier phenolic foam article of claim 1, wherein: the cell opener is AES, sodium dodecyl benzene sulfonate and detergent.
7. A method for preparing the nitrogen-oxygen separation carrier phenolic foam product as defined in any one of claims 1 to 6, wherein the method comprises the following steps: the method comprises the following steps:
step one, putting high-performance phenolic resin, a foaming agent, a wetting agent, a pore-forming agent, ethanol, butanol and sodium butoxide into a stirring tank according to a proportion, stirring, and uniformly mixing for later use;
step two, conveying the mixture to a pouring head through a conveying pipe, quickly and uniformly stirring the mixture and a curing agent in the other conveying pipe, pouring the mixture into a heated laminating machine, and laminating;
and step three, sending the material to a drying room, and carrying out rising, curing, forming and demoulding to obtain the nitrogen-oxygen separation carrier phenolic foam product.
8. The method for producing according to claim 7, characterized in that: recyclable plastic films are paved on the upper surface and the lower surface of the laminating machine.
9. The method of claim 7, wherein: the temperature of the drying room is 75-85 ℃, the length of the production line of the drying device is 18 meters, and the speed of the chain plate is 1.2-1.5 m/s.
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| CN201910824758.XA CN110498999B (en) | 2019-09-02 | 2019-09-02 | Nitrogen-oxygen separation carrier phenolic foam product and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4575521A (en) * | 1984-10-30 | 1986-03-11 | Exxon Research And Engineering Company | Closed cell phenolic foams |
| CN1942496A (en) * | 2004-04-23 | 2007-04-04 | 恩琪斯化学公司 | Novel phenolic resins |
| CN102558757A (en) * | 2011-12-30 | 2012-07-11 | 福建天利高新材料有限公司 | Neutral obturator phenolic aldehyde foam plastic and preparation method thereof |
| CN102765201A (en) * | 2012-07-24 | 2012-11-07 | 苏州浩海节能环保材料有限公司 | Continuous processing production line of foamed phenolic insulation boards |
-
2019
- 2019-09-02 CN CN201910824758.XA patent/CN110498999B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4575521A (en) * | 1984-10-30 | 1986-03-11 | Exxon Research And Engineering Company | Closed cell phenolic foams |
| CN1942496A (en) * | 2004-04-23 | 2007-04-04 | 恩琪斯化学公司 | Novel phenolic resins |
| CN102558757A (en) * | 2011-12-30 | 2012-07-11 | 福建天利高新材料有限公司 | Neutral obturator phenolic aldehyde foam plastic and preparation method thereof |
| CN102765201A (en) * | 2012-07-24 | 2012-11-07 | 苏州浩海节能环保材料有限公司 | Continuous processing production line of foamed phenolic insulation boards |
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