CN114656671B - Preparation method of composite straw-based degradable waste polyurethane foam wall material - Google Patents
Preparation method of composite straw-based degradable waste polyurethane foam wall material Download PDFInfo
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- CN114656671B CN114656671B CN202210471909.XA CN202210471909A CN114656671B CN 114656671 B CN114656671 B CN 114656671B CN 202210471909 A CN202210471909 A CN 202210471909A CN 114656671 B CN114656671 B CN 114656671B
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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
- C08J9/06—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
- C08J9/08—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 carbon dioxide
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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
- C08J9/143—Halogen containing compounds
- C08J9/144—Halogen containing compounds containing carbon, halogen and hydrogen only
- C08J9/145—Halogen containing compounds containing carbon, halogen and hydrogen only only chlorine as halogen atoms
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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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
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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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
- C08J2203/142—Halogenated saturated hydrocarbons, e.g. H3C-CF3
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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
- C08J2397/00—Characterised by the use of lignin-containing materials
- C08J2397/02—Lignocellulosic material, e.g. wood, straw or bagasse
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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
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
- C08J2475/08—Polyurethanes from polyethers
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- 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
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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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)
- General Chemical & Material Sciences (AREA)
- Polyurethanes Or Polyureas (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention discloses a preparation method of a composite straw-based degradable waste polyurethane foam wall material, and relates to the field of building materials. The method comprises the following steps: crushing straw stalks, then placing the crushed straw stalks in an alkaline solution 1, and sequentially mixing the crushed straw stalks with phenol and formaldehyde for modification reaction to obtain modified straw fine aggregate; modifying the waste polyurethane foam plastics; mixing the modified straw fine aggregate and the modified polyurethane foam powder solution to obtain a mixed solution; and mixing and stirring the mixed solution with polyether polyol, a foam stabilizer, an alcohol amine catalyst, a metal catalyst, a physical foaming agent and a chemical foaming agent, adding isocyanate, stirring, standing and foaming to obtain the composite straw-based degradable waste polyurethane foam wall material. The invention ensures the low density of the degradable straw-based polyurethane foam wall material and further improves the mechanical and heat-insulating properties of the degradable straw-based polyurethane foam wall material.
Description
Technical Field
The invention relates to the field of building materials, in particular to a preparation method of a composite straw-based degradable waste polyurethane foam wall material.
Background
The degradable straw-based polyurethane foam wall material has the advantages of low density, low heat conductivity coefficient, degradability, greenness, no pollution, convenience in construction and the like, and has application in the field of building external wall thermal insulation materials. As a thermal insulation material for building external walls, the degradable straw-based polyurethane foam wall material needs to be further improved in mechanical and thermal insulation properties while ensuring low density.
Disclosure of Invention
Based on the above discussion, the invention provides a preparation method of a composite straw-based degradable waste polyurethane foam wall material, which can further improve the mechanical and heat-insulating properties of the degradable straw-based polyurethane foam wall material while ensuring the low density of the degradable straw-based polyurethane foam wall material.
In order to achieve the purpose, the invention provides the following scheme:
the invention discloses a preparation method of a composite straw-based degradable waste polyurethane foam wall material, which comprises the following steps:
crushing straw stalks, then placing the crushed straw stalks in an alkaline solution, and mixing the crushed straw stalks with phenol and formaldehyde in sequence for modification reaction to obtain modified straw fine aggregate;
ball-milling and crushing the waste polyurethane foam plastic, mixing the crushed waste polyurethane foam plastic with ethylene glycol and sodium hydroxide powder, stirring to obtain a mixed solution, adding the ball-milled and crushed waste polyurethane foam plastic into the mixed solution, and stirring to obtain a modified polyurethane foam plastic powder solution;
mixing the modified straw fine aggregate and the modified polyurethane foam powder solution to obtain a mixed solution;
and mixing and stirring the mixed solution with polyether polyol, a foam stabilizer, an alcohol amine catalyst, a metal catalyst, a physical foaming agent and a chemical foaming agent, adding isocyanate, stirring, standing and foaming to obtain the composite straw-based degradable waste polyurethane foam wall material.
The straw stalk is modified to contain a great amount of natural renewable polymer material-lignin, a great amount of groups such as conjugated double bonds, aromatic groups, methoxy groups, carbonyl groups, hydroxyl groups and the like exist in the structure of the lignin, but the activity is low, phenol and formaldehyde are used for phenolization and hydroxymethylation modification under the alkali catalysis condition, the content of the hydroxyl groups in the lignin is increased, the reaction activity of the lignin is improved, and partial polyalcohol is replaced to participate in chemical reaction, so that the mechanical and heat insulation properties of the polyurethane foam wall material are improved.
The waste polyurethane foam plastic is modified by using ethylene glycol as an alcoholysis agent, and the crushed polyurethane foam is subjected to alcoholysis at a certain temperature to partially replace polyol to prepare rigid polyurethane foam, so that the mechanical and heat-insulating properties of the prepared waste polyurethane foam wall material are improved.
Furthermore, the fineness modulus of the crushed straw stalks is 2.5-3.0.
Further, the alkaline solution is a sodium hydroxide solution with the concentration of 0.1 mol/L.
Further, the conditions of the modification reaction are specifically as follows: pH is 9-12, temperature is 80-110 deg.C, and time is 1-3 h.
Further, the straw stalk after modification reaction also comprises the steps of adjusting the pH value to 2-3, washing with deionized water, vacuum filtering to neutrality, and vacuum drying at 60-80 ℃ for 4-6 h.
Further, the mass ratio of the straw stalks to the phenol and the formaldehyde is 30-40: 60-80: 45-60.
Further, the mass ratio of the sodium hydroxide powder to the waste polyurethane foam plastic is 0.03-0.07: 1.
Further, the mass ratio of the waste polyurethane foam plastic to the ethylene glycol is 2-4: 10.
Further, the mass ratio of the modified straw fine aggregate to the modified polyurethane foam plastic powder in the mixed liquid is 30-40: 10-20.
Further, the mass ratio of the mixing liquid to the polyether polyol, the foam stabilizer, the alcohol amine catalyst, the metal catalyst, the physical foaming agent, the chemical foaming agent and the isocyanate is 0.9-1:3.8-4.2:0.049-0.051:0.029-0.031:0.044-0.046:0.49-0.51:0.0420-0.425: 3.8-4.2.
Further, the polyether polyol is polyether polyol 4110, and the hydroxyl value is 450 +/-20 mgKOH/g; the foam stabilizer is dimethyl silicone oil, the alcohol amine catalyst is triethanolamine, the metal catalyst is dibutyltin dilaurate, the physical foaming agent is dichloromethane, and the chemical foaming agent is water.
The invention discloses the following technical effects:
the invention firstly modifies the straw fine aggregate under alkaline condition, and then mixes the modified straw fine aggregate with the modified waste polyurethane foam, polyether glycol, isocyanate and the like to prepare the straw-based degradable waste polyurethane foam wall material, thereby realizing that the density of the waste polyurethane foam wall material reaches 42kg/m 3 The compression strength reaches 0.62MPa, the heat conductivity coefficient is 0.020W/(m.k), compared with the waste polyurethane foam wall material without straw-based aggregate, the mechanical and heat-insulating properties of the straw-based waste polyurethane foam are improved, and simultaneously, the biomass energy is realizedThe source is utilized, the straw-based waste polyurethane foam is easy to degrade in natural environment, and the pollution to the environment can be reduced.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but rather as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated herein by reference to disclose and describe the methods and/or materials in connection with which the documents are cited. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The "parts" in the present invention are all parts by mass unless otherwise specified.
The "room temperature" in the examples of the present invention means 15 to 30 ℃ unless otherwise specified.
The rice straw used in the embodiment of the invention is common rice straw in the three provinces of northeast China, and before modification treatment, the rice straw is firstly aired in natural light for 3 days. Then, a common 380V three-phase electric hay cutter is used for cutting fine aggregates with the length of 1-2 CM under a particle size particle screening machine, and the fine aggregates with the fineness modulus of 2.5-3.0 are prepared by screening through a square hole sieve.
Example 1
Step 1, preparing modified straw fine aggregate: taking 35 parts of straw fine aggregate, drying until the water content is less than 13%, placing the dried straw fine aggregate into a three-neck flask with a condenser and a thermometer, dropwise adding 0.1mol/L sodium hydroxide solution to adjust the pH value to 10, adding 70 parts of phenol into the three-neck flask, and uniformly stirring to obtain a mixed solution. Placing the three-neck flask into a water bath kettle with a stirrer, stirring for 1h in a constant-temperature water bath at the temperature of 80 ℃, dropwise adding 52 parts of formaldehyde into the three-neck flask, continuing stirring for 1h in the constant-temperature water bath, pouring the solution into 100 parts of distilled water, cooling to room temperature, adding HCl to adjust the pH value to 3.0, washing with deionized water, carrying out vacuum filtration to neutrality, and placing in an oven for vacuum drying for 4h at the temperature of 60 ℃ to obtain the modified straw fine aggregate.
Step 2, preparing a modified polyurethane foam powder solution: placing a three-neck flask with a condenser pipe and a thermometer in a 0 ℃ oil bath, adding 100 parts of ethylene glycol and 10 parts of waste polyurethane foam plastic powder crushed by a ball mill into the three-neck flask, heating to 180 ℃, adding 1g of 96% mass fraction sodium hydroxide powder, stirring at a high speed of 4500r/min for 1h, adding 10 parts of waste polyurethane foam powder crushed by a ball mill into the three-neck flask, continuing to stir at a high speed at 180 ℃ and 4500r/min for 1h, and then ventilating and cooling to room temperature to obtain the modified polyurethane foam plastic powder solution.
And 3, mixing the modified straw fine aggregate prepared in the step 1 with the modified polyurethane foam plastic powder solution prepared in the step 2, and uniformly mixing to obtain a mixed solution. Mixing 4 parts of the mixed solution with 16 parts of polyether polyol 4110, 0.2 part of dimethyl silicone oil, 0.12 part of triethanolamine, 0.18 part of dibutyltin dilaurate, 2 parts of dichloromethane and 0.17 part of water to obtain a white material, stirring the white material at a high speed for 10s under the condition of 4500r/min, adding 16 parts of isocyanate into the white material, continuously stirring for 15s under the condition of 4500r/min, and standing and foaming for 30s to obtain the composite straw-based degradable waste polyurethane foam wall material.
The composite straw-based degradable waste polyurethane foam wall material prepared in the embodiment is subjected to performance detection, and the detection standards refer to GB/T6343-.
The result shows that the apparent density of the composite straw-based degradable waste polyurethane foam wall material prepared by the embodiment is 42kg/m 3 The apparent density of the common foam concrete wall thermal insulation material is generally 500-1000kg/m 3 The dead weight of a building heat-insulating wall structure with the same design is at least reduced by 91.6 percent, the compression strength is 0.62MPa, the heat conductivity coefficient is 0.020W/(m.k), the heat conductivity coefficient of the foam concrete wall heat-insulating material is generally 0.15-0.5W/(m.k), and the heat-insulating property of the composite straw-based degradable waste polyurethane foam wall material is far superior to that of the foam concrete wall heat-insulating material. The straw-based waste polyurethane foam wall material improves the mechanical and heat-insulating properties thereof, realizes the utilization of biomass energy, and the degradable waste polyurethane foam wall material added with the straw-based aggregate is easy to degrade in natural environment, so that the pollution to the environment can be reduced.
Comparative example 1
The same as in example 1, except that the step of modifying straw fine aggregate in step 1 was omitted, and straw fine aggregate which was not modified in step 3 was directly mixed with the modified polyurethane foam powder solution prepared in step 2.
The same test as in example 1 was performed on the degradable waste polyurethane foam wall material prepared in this comparative example. The result shows that the compressive strength of the degradable waste polyurethane foam wall material prepared by the comparative example is 0.43MPa, the thermal conductivity coefficient is 0.024W/(m.k), and compared with the degradable waste polyurethane foam with the modified straw-based aggregate, the mechanical and thermal insulation properties of the degradable waste polyurethane foam with the unmodified straw-based aggregate are reduced because lignin is not subjected to hydroxymethylation activation, the material flowability is influenced, the foaming is influenced, the distribution of a cellular structure is uneven, and macropores, defect structures and the like are generated, so that the closed cell rate is reduced, and the thermal conductivity coefficient is increased.
Comparative example 2
Same as example 1 except that step 1 was omitted; in step 3, the addition of straw fine aggregate is omitted.
The same test as in example 1 was performed on the degradable waste polyurethane foam wall material prepared in this comparative example. The result shows that the degradable waste polyurethane foam wall material prepared by the comparative example has the compression strength of 0.31MPa and the thermal conductivity coefficient of 0.022W/(m.k), and compared with the degradable waste polyurethane foam wall material added with the modified straw-based aggregate, the mechanical and heat-insulating properties of the degradable waste polyurethane foam wall material without the straw-based aggregate are reduced, and meanwhile, the degradation difficulty of the waste polyurethane foam wall material is improved by the wall material without the biomass energy straw-based aggregate.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (2)
1. A preparation method of a composite straw-based degradable waste polyurethane foam wall material is characterized by comprising the following steps:
crushing straw stalks, then placing the crushed straw stalks in an alkaline solution, and sequentially mixing the crushed straw stalks with phenol and formaldehyde for modification reaction to obtain modified straw fine aggregate;
ball-milling and crushing waste polyurethane foam plastics, mixing the crushed waste polyurethane foam plastics with ethylene glycol and sodium hydroxide powder, stirring to obtain a mixed solution, adding the ball-milled and crushed waste polyurethane foam plastics into the mixed solution, and stirring to obtain a modified polyurethane foam plastic powder solution;
mixing the modified straw fine aggregate with the modified polyurethane foam powder solution to obtain a mixed solution;
mixing and stirring the mixed solution with polyether polyol, a foam stabilizer, an alcohol amine catalyst, a metal catalyst, a physical foaming agent and a chemical foaming agent, adding isocyanate, stirring, standing and foaming to obtain the composite straw-based degradable waste polyurethane foam wall material;
the fineness modulus of the crushed straw stalks is 2.5-3.0;
the alkaline solution is a sodium hydroxide solution with the concentration of 0.1 mol/L;
the conditions of the modification reaction are specifically as follows: the pH value is 9-12, the temperature is 80-110 ℃, and the time is 1-3 h;
the rice straw also comprises the steps of adjusting the pH value to 2-3 after modification reaction, washing with deionized water, vacuum-filtering to neutrality, and vacuum-drying at 60-80 ℃ for 4-6 h;
the mass ratio of the straw stalk to the phenol to the formaldehyde is (30-40: 40-80): 45-60 parts of;
the mass ratio of the sodium hydroxide powder to the waste polyurethane foam plastic is 0.03-0.07: 1;
the mass ratio of the modified straw fine aggregate to the modified polyurethane foam plastic powder in the mixed liquid is 30-40: 10-20;
the polyether polyol is 4110, and the hydroxyl value is 450 +/-20 mgKOH/g; the foam stabilizer is dimethyl silicone oil, the alcohol amine catalyst is triethanolamine, the metal catalyst is dibutyltin dilaurate, the physical foaming agent is dichloromethane, and the chemical foaming agent is water.
2. The preparation method of the composite straw-based degradable waste polyurethane foam wall material as claimed in claim 1, wherein the mass ratio of the mixing liquid to the polyether polyol, the foam stabilizer, the alcohol amine catalyst, the metal catalyst, the physical foaming agent, the chemical foaming agent and the isocyanate is 0.9-1:3.8-4.2:0.049-0.051:0.029-0.031:0.044-0.046:0.49-0.51:0.0420-0.430: 3.8-4.2.
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| CN102585142B (en) * | 2011-01-14 | 2013-09-04 | 中国林业科学研究院木材工业研究所 | Biomass polyurethane foam and method for preparing same |
| CN103224628B (en) * | 2013-05-24 | 2015-03-25 | 济南圣泉集团股份有限公司 | Hydroxymethylated lignin and application thereof |
| CN103849135A (en) * | 2014-03-04 | 2014-06-11 | 北华大学 | Preparation method of degradable polyurethane foaming plastic |
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