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CN106700119B - Blowing agent composition and polyurethane rigid foam - Google Patents

Blowing agent composition and polyurethane rigid foam Download PDF

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Publication number
CN106700119B
CN106700119B CN201611220158.5A CN201611220158A CN106700119B CN 106700119 B CN106700119 B CN 106700119B CN 201611220158 A CN201611220158 A CN 201611220158A CN 106700119 B CN106700119 B CN 106700119B
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parts
mass
lba
agent composition
foam
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CN106700119A (en
Inventor
戴建斌
李鹏
贾振飞
王海娟
朱小兵
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Qingdao Haier Refrigerator Co Ltd
Haier Smart Home Co Ltd
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Qingdao Haier Co Ltd
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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
    • C08J9/149—Mixtures of blowing agents covered by more than one of the groups C08J9/141 - C08J9/143
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4804—Two or more polyethers of different physical or chemical nature
    • C08G18/4816—Two or more polyethers of different physical or chemical nature mixtures of two or more polyetherpolyols having at least three hydroxy groups
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2110/00—Foam properties
    • C08G2110/0025—Foam properties rigid
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2110/00—Foam properties
    • C08G2110/0041—Foam properties having specified density
    • C08G2110/005—< 50kg/m3
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/16—Unsaturated hydrocarbons
    • C08J2203/162—Halogenated unsaturated hydrocarbons, e.g. H2C=CF2
    • 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
    • C08J2203/18—Binary blends of expanding agents
    • C08J2203/182—Binary blends of expanding agents of physical blowing agents, e.g. acetone and butane
    • 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
    • C08J2205/00—Foams characterised by their properties
    • C08J2205/04—Foams characterised by their properties characterised by the foam pores
    • C08J2205/052—Closed cells, i.e. more than 50% of the pores are closed
    • 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
    • C08J2205/00—Foams characterised by their properties
    • C08J2205/10—Rigid foams
    • 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
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • C08J2375/08—Polyurethanes from polyethers

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Refrigerator Housings (AREA)

Abstract

The invention discloses a foaming agent composition and polyurethane rigid foam, wherein the foaming agent composition comprises the following components: 12.5-13.5 parts by mass of cyclopentane; and LBA 2 ~ 3 parts by mass. Compared with the prior art, the formula of the foaming agent is improved, the LBA is increased on the basis of cyclopentane, the density and the heat conductivity coefficient of the heat insulation foam are reduced on the basis of ensuring the improvement of the performance of the heat insulation foam of the refrigerator, the foaming cost of the refrigerator is effectively saved, the performance of the foam is improved, and the energy consumption of the refrigerator is further effectively reduced.

Description

Blowing agent composition and polyurethane rigid foam
Technical Field
The invention relates to the technical field of foaming heat-insulating materials, in particular to a foaming agent composition and polyurethane rigid foam.
Background
The heat insulation material of the traditional refrigerator body is basically formed by independently using cyclopentane as a foaming agent and combining polyether and isocyanate to complete foaming, the formed polyurethane rigid foam has high density and relatively high heat conductivity coefficient, and the density and the heat conductivity coefficient are difficult to reduce by adjusting the formula. At the same time, it is difficult to ensure that other properties of the insulating foam change, so that the desired requirements of the user cannot be effectively met.
Disclosure of Invention
The invention aims to solve at least one technical problem in the prior art and provides a foaming agent composition capable of reducing the density and the thermal conductivity of a heat insulation foaming layer of a refrigerator.
The invention also aims to provide a polyurethane rigid foam with low thermal conductivity.
Wherein, a foaming agent composition comprises:
12.5-13.5 parts by mass of cyclopentane; and
LBA 2 ~ 3 parts by mass.
As a further improvement of the present invention, a blowing agent composition comprising:
13 parts by mass of cyclopentane; and
LBA 2.5 parts by mass.
To achieve still another object of the present invention, there is provided a rigid polyurethane foam comprising:
100 parts of combined polyether;
137-141 parts by mass of isocyanate;
15 to 16 parts by mass of the blowing agent composition.
As a further improvement of the present invention, a rigid polyurethane foam comprises:
100 parts of combined polyether;
139 parts by mass of isocyanate;
15.5 parts by mass of the blowing agent composition claimed in claim 1 or 2.
As a further improvement of the invention, the combined polyether is prepared by mixing the following raw materials:
60 parts by mass of polyether polyol with the average functionality of 4.9 and the hydroxyl value of 400-450 mgKOH/g;
30 parts by mass of polyether polyol with the average functionality of 3.7 and the hydroxyl value of 470-480 mgKOH/g;
crosslinking agent R350X 5 parts by mass;
2 parts by mass of a foam stabilizer;
0.9 part by mass of water;
1.4 parts by mass of a composite catalyst; and
and 8 parts of a flame retardant.
As a further improvement of the invention, the composite catalyst is a composite catalyst of tertiary amine and organic tin.
As a further development of the invention, the foam stabilizer is an organosilicon compound.
As a further improvement of the invention, the flame retardant is an organophosphate.
As a further improvement of the present invention, the LBA is HCFO-1233zd trifluoropropene.
Compared with the prior art, the formula of the foaming agent is improved, the LBA is increased on the basis of cyclopentane, the density and the heat conductivity coefficient of the heat insulation foam are reduced on the basis of ensuring the improvement of the performance of the heat insulation foam of the refrigerator, the foaming cost of the refrigerator is effectively saved, the performance of the foam is improved, and the energy consumption of the refrigerator is further effectively reduced.
Drawings
FIG. 1 is an SEM photograph of cells of a rigid polyurethane foam using only cyclopentane as a blowing agent in one embodiment of the present invention;
FIG. 2 is an SEM photograph of cells of a rigid polyurethane foam using cyclopentane/LBA as the blowing agent in one embodiment of the present invention.
Detailed Description
The present invention will be described in detail below. These embodiments are not intended to limit the present invention, and structural, methodological, or functional changes made by those skilled in the art according to these embodiments are included in the scope of the present invention. Variations in reaction conditions, amounts of reactants or starting materials, which may be made by one of ordinary skill in the art in light of these examples, are within the scope of the invention.
The blowing agent composition of the present invention comprises: 12.5 to 13.5 parts by mass of cyclopentane (cp); 2 to 3 parts by mass of LBA.
Wherein LBA is HCFO-1233zd trifluoropropene, a new generation liquid foaming agent.
Physical Properties of LBA
Molecular formula C3H2ClF3
Molecular weight 130.50
Boiling point,. degree.C 20
Specific gravity (25 ℃), g/cm3 1.312
Flash point, DEG C -10
ODP ≈0
GWP 4.7-7
Quality index of LBA
Appearance of the product Colorless transparent liquefied gas
Purity% ≥99.5
Water content, mg/kg ≤100
The formula of the existing foaming agent is improved, a proper amount of LBA is added on the basis of cyclopentane, and the density and the heat conductivity coefficient of a foaming body material are reduced through the blending of a multi-element foaming agent on the basis of ensuring the improvement of the heat insulation foam performance of a refrigerator, so that the energy consumption of the refrigerator is reduced, and the foaming cost is reduced.
In a preferred embodiment of the present invention, the blowing agent composition comprises: 13 qualityAmounts of cyclopentane (cp) and 2.5 parts by mass of LBA, a blowing system using the blowing agent composition that can reduce the thermal conductivity from 19.8mw/m.k for cyclopentane (cp) foam to 18.40mw/m.k for the foam and a density of 36 Kg/m.k for cyclopentane (cp) system3Reduced to 32Kg/m of the foam material3The refrigerator foaming cost is effectively saved, the performance of the foam is improved, and the energy consumption of the refrigerator is effectively reduced.
The foaming agent composition is mainly suitable for a polyurethane rigid foam foaming system taking polyether polyol as a base material, and the prepared polyurethane rigid foam is particularly suitable for heat insulation of household electrical appliances such as refrigerators, freezers, water heaters, cooked rice pots and the like, and can also be used for freezing and refrigerating equipment such as refrigerated trucks, freezing containers, storage tanks, cold storages and the like.
The invention also provides polyurethane rigid foam prepared by using the foaming agent composition of the embodiment of the invention. The rigid polyurethane foam may include 100 parts by mass of a conjugate polyether; 137 to 141 parts by mass of an isocyanate; and 15 to 16 parts by mass of the foaming agent composition. The invention can further reduce the density of the rigid polyurethane foam by limiting the content of each component of the rigid polyurethane foam and selecting the component content which is more suitable for the foaming agent composition of the invention.
Preferably, in the present embodiment, the polyurethane rigid foam includes 100 parts by mass of the conjugate polyether; 139 parts by mass of an isocyanate; and 15.5 parts by mass of the aforementioned blowing agent composition.
Table 1 shows the components and proportions of the conjugate polyether according to specific embodiments of the present invention. Wherein, the foam stabilizer, the composite catalyst, the flame retardant and the like can be selected from common reagents in the technical field. For example, the composite catalyst can be selected from composite catalysts of tertiary amines and organic tin. The foam stabilizer can be selected from organosilicon compounds or organosilicon compounds, and the main structure of the foam stabilizer is as follows: a polysiloxane-alkylene oxide block copolymer. The flame retardant may be selected from organic phosphates. The inventors of the present application have creatively found that the conjugate polyethers shown in table 1 are more suitable for the blowing agent composition of the present invention than conjugate polyethers having other components and ratios. That is, the rigid polyurethane foam prepared using the blowing agent composition of the present invention, the conjugate polyether shown in Table 1, and the formulation of the present invention has better properties.
TABLE 1
Figure BDA0001192618240000051
Table 2 shows parameter information of components, compounding ratios, and raw materials of the rigid polyurethane foam according to one embodiment of the present invention. See table 2, wherein the conjugate polyether is selected according to the components and proportions in table 1.
TABLE 2
Figure BDA0001192618240000052
In the embodiment of the invention, the storage temperature of the combined polyether is generally 15-23 ℃. During foaming, the combined polyether and the foaming agent composition are conveyed into a premixing chamber for premixing, then mixed with isocyanate, and injected into a mold cavity by using a high-pressure foaming machine to complete foaming and filling. Specific process parameters can be found in table 3.
TABLE 3
Figure BDA0001192618240000061
Table 4 shows a foaming process according to one specific embodiment of the present invention.
TABLE 4
Figure BDA0001192618240000062
The foam physical properties of the foaming system using the CP/LBA component as the blowing agent are shown in Table 5, which are greatly improved mainly in terms of density, thermal conductivity and cell size of the foam.
The polyurethane foaming system comprises the following main components in percentage by weight:
the mass portions of the combined polyether are as follows: 100
Isocyanate mass portion: 136
The Cyclopentane (CP) foaming agent comprises the following components in parts by mass: 13
LBA foaming agent mass portion: 2.5
TABLE 5
Figure BDA0001192618240000071
In contrast, in the prior art, the foam physical properties of the foaming system using only the CP component as a blowing agent are shown in Table 6.
The proportion of each main component of the polyurethane foaming system is as follows:
the mass portion of the combined polyether polyol is as follows: 100
Isocyanate mass portion: 141
The Cyclopentane (CP) foaming agent comprises the following components in parts by mass: 13.
TABLE 6
Figure BDA0001192618240000072
Figure BDA0001192618240000081
As can be seen from a comparison of the test results in tables 5 and 6, the physical properties of the rigid polyurethane foam using the CP/LBA blowing agent composition system are greatly improved, mainly in terms of density, thermal conductivity, and foam cell size. In the invention, as the LBA is additionally added in the original CP (cyclopentane) foaming system, and the proportion of the LBA and the CP is optimized (13/2.5 of the LBA), the flowability of the foaming system material is increased, and the heat conductivity coefficient of the polyurethane rigid foam is greatly reduced. Specifically, the thermal conductivity of the rigid polyurethane foam is reduced from about 19.8mw/m.k of a common cp foaming system to about 18.4mw/m.k, and the overall density is 36 Kg/m.k of a cp foaming agent system3Reduced to 30Kg/m of CP/LBA blowing agent system3Left and right; variation of cell Range As shown in FIGS. 1 and 2, the cell size of the CP/LBA blowing agent system is smaller and more uniform。
According to the invention, through the blending of the CP/LBA foaming agent, the density and the heat conductivity coefficient of the polyurethane rigid foam are reduced on the basis of ensuring the improvement of the performance of the polyurethane rigid foam. The polyurethane rigid foam provided by the embodiment of the invention is particularly suitable for a refrigerator, can effectively save the foaming cost of the refrigerator and improve the performance of the foam, and further effectively reduces the energy consumption of the refrigerator.
It should be understood that although the present description refers to embodiments, not every embodiment contains only a single technical solution, and such description is for clarity only, and those skilled in the art should make the description as a whole, and the technical solutions in the embodiments can also be combined appropriately to form other embodiments understood by those skilled in the art.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.

Claims (7)

1. A rigid polyurethane foam, comprising:
100 parts of combined polyether;
137-141 parts by mass of isocyanate;
15-16 parts by mass of a foaming agent composition;
the composite polyether is prepared by mixing the following raw materials:
60 parts by mass of polyether polyol with the average functionality of 4.9 and the hydroxyl value of 400-450 mgKOH/g;
30 parts by mass of polyether polyol with the average functionality of 3.7 and the hydroxyl value of 470-480 mgKOH/g;
crosslinking agent R350X 5 parts by mass;
2 parts by mass of a foam stabilizer;
0.9 part by mass of water;
1.4 parts by mass of a composite catalyst; and
8 parts of a flame retardant;
the blowing agent composition employs a cyclopentane/LBA component as the blowing agent, wherein,
12.5-13.5 parts by mass of cyclopentane; and
LBA 2 ~ 3 parts by mass.
2. The rigid polyurethane foam according to claim 1, wherein the blowing agent composition uses a cyclopentane/LBA component as the blowing agent, wherein,
13 parts by mass of cyclopentane; and
LBA 2.5 parts by mass.
3. The rigid polyurethane foam according to claim 1, comprising:
100 parts of combined polyether;
139 parts by mass of isocyanate;
15.5 parts by mass of the blowing agent composition.
4. The rigid polyurethane foam according to claim 1,
the composite catalyst is a composite catalyst of tertiary amine and organic tin.
5. The rigid polyurethane foam according to claim 1, wherein the foam stabilizer is an organosilicon compound.
6. The rigid polyurethane foam according to claim 1, wherein the flame retardant is an organophosphate.
7. The rigid polyurethane foam according to claim 1, wherein the LBA is HCFO-1233zd trifluoropropene.
CN201611220158.5A 2016-12-26 2016-12-26 Blowing agent composition and polyurethane rigid foam Active CN106700119B (en)

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MX2019014811A (en) * 2017-06-13 2020-02-10 Honeywell Int Inc Improved foam formulation.
CN108250404A (en) * 2017-12-28 2018-07-06 青岛海尔股份有限公司 Polyurethane rigid foam plastic and preparation method thereof
CN108192065A (en) * 2017-12-28 2018-06-22 青岛海尔股份有限公司 Polyurethane rigid foam plastic and preparation method thereof

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CN104672420A (en) * 2015-02-09 2015-06-03 万华化学（宁波）容威聚氨酯有限公司 High-strength polyurethane rigid foam as well as preparation method and application thereof
CN106188615A (en) * 2015-05-04 2016-12-07 青岛海尔特种电冰柜有限公司 Triple combination foaming agent, hard polyurethane foam and manufacture method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104672420A (en) * 2015-02-09 2015-06-03 万华化学（宁波）容威聚氨酯有限公司 High-strength polyurethane rigid foam as well as preparation method and application thereof
CN106188615A (en) * 2015-05-04 2016-12-07 青岛海尔特种电冰柜有限公司 Triple combination foaming agent, hard polyurethane foam and manufacture method thereof

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