CN110951022A - Conjugate polyether for manufacturing glass fiber composite material and preparation method and application thereof - Google Patents
Conjugate polyether for manufacturing glass fiber composite material and preparation method and application thereof Download PDFInfo
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- CN110951022A CN110951022A CN201911309903.7A CN201911309903A CN110951022A CN 110951022 A CN110951022 A CN 110951022A CN 201911309903 A CN201911309903 A CN 201911309903A CN 110951022 A CN110951022 A CN 110951022A
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- 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
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- 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
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
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- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4205—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups
- C08G18/4208—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups
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- 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
- C08G18/4812—Mixtures of polyetherdiols with polyetherpolyols having at least three hydroxy groups
-
- 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
- C08G18/4829—Polyethers containing at least three hydroxy groups
-
- 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
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
-
- 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
- C08G2110/0083—Foam properties prepared using water as the sole blowing agent
-
- 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
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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)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention belongs to the technical field of high polymer materials, and particularly relates to composite polyether for manufacturing a glass fiber composite material, and a preparation method and application thereof. The combined polyether for manufacturing the glass fiber composite material is prepared from polyether polyol A, polyether polyol B, polyester polyol C, a foam stabilizer, a foaming agent, a catalyst, a flame retardant and a coloring agent; according to the invention, by optimizing the formula structure and performance of the polyether product, the polyurethane material with excellent quality can be produced only by using the standardized isocyanate product, and can be compounded with glass fiber materials with various sizes and structures, so that the final product has good heat insulation performance and specific strength.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to composite polyether for manufacturing a glass fiber composite material, and a preparation method and application thereof.
Background
Polyurethane foam is a high molecular material with good processability. The combined polyether product (also called polyurethane combined material) is a forming process route for forming a polyurethane material by mixing combined polyether (including polyether polyol, polyester polyol, a catalyst, a foaming agent, a stabilizer and other structural auxiliaries) and polyisocyanate in a certain proportion and then reacting and forming.
At present, polyol and isocyanate required by polyurethane molding are mostly divided into A, B components by high-end heat insulation materials and functional polyurethane materials, wherein the B component polyisocyanate is often specially modified, so that part of special properties of final products are improved. The corresponding process and formula are relatively complicated, and the production cost is high.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the preparation method comprises the steps of optimizing the formula structure and performance of a polyether product, and only using a standardized isocyanate product to produce a polyurethane material with excellent quality, wherein the polyurethane material can be compounded with glass fiber materials with various sizes and structures, so that a final product has good heat insulation performance and specific strength.
The combined polyether for manufacturing the glass fiber composite material is prepared from the following raw materials in percentage by mass:
wherein the polyether polyol A is polypropylene oxide polyether polyol with average functionality of 3-6 and molecular weight of 300-1000; the polyether polyol B is polypropylene oxide polyether polyol with average functionality of 2-4 and molecular weight of 500-2000; the polyester polyol C is phthalic anhydride aromatic polyester polyol with average functionality of 2, hydroxyl value of 300-500 mgKOH/g and molecular weight of 200-400.
The foam stabilizer is a Si-C surfactant. Preferably L6950 from Michigan high and New materials group or JC7750 from Cangzhou Junchi industries, chemical Co.
The foaming agent is deionized water.
The catalyst is an organic amine catalyst and/or an organic metal catalyst. Wherein, the organic amine catalyst can be selected from: n, N-dimethylcyclohexylamine, N-dimethylbenzylamine, N-dimethyl-propylene-hexahydrotriazine; the organic metal catalyst is selected from dibutyltin dilaurate, potassium acetate and potassium isooctanoate.
When the catalyst is a mixture of an organic amine catalyst and an organic metal catalyst, the mass ratio of the organic amine catalyst to the organic metal catalyst is 1: 3-3: 1.
The flame retardant is a phosphate ester additive flame retardant. The method comprises the following steps of adopting a mixture of tris (2-chloropropyl) phosphate and triethyl phosphate, wherein the mass ratio of the tris (2-chloropropyl) phosphate to the triethyl phosphate is 1: 3-3: 1.
The colorant is used for controlling the color of the product and is selected according to the color requirement of the final product.
The preparation method of the combined polyether for manufacturing the glass fiber composite material comprises the following steps: and (2) putting the weighed polyether polyol A, polyether polyol B and polyester polyol C into a reaction kettle, stirring, then adding the weighed catalyst, foaming agent, foam stabilizer, flame retardant and colorant, stirring for 30 minutes to 1 hour, sampling, detecting, and packaging after the materials are qualified.
The application of the combined polyether for manufacturing the glass fiber composite material is that the combined polyether for manufacturing the glass fiber composite material and polyisocyanate are mixed and reacted according to the mass ratio of 1: 1.2-1: 2.2, then the mixed polyether is distributed on a base material containing glass fiber, and the glass fiber composite material with good specific strength can be obtained after molding through a mold.
The polyisocyanate is diphenylmethane diisocyanate and/or polyphenyl methane polyisocyanate.
The glass fiber composite material prepared by the invention has the following product performance indexes after detection:
density of finished products: 100 to 700kg/m3；
Glass fiber plane compressive strength: 0.5 to 20 MPa;
closed pore rate: 20-90%;
oxygen index: is greater than 26.
Compared with the prior art, the invention has the following beneficial effects:
1. the polyether composition for manufacturing the glass fiber composite material has good heat insulation performance and specific strength of a final product by optimizing the reasonable collocation of the polyether polyol, the polyester polyol and the compound auxiliary agent.
2. The flame-retardant coating has good flame-retardant performance and can be used for mobile vehicle interior devices such as automobiles, motor homes and the like.
3. The raw materials adopted by the invention are green and environment-friendly, and the final material has low VOC content and no odor by optimizing the matching of the auxiliary agents.
4. The composite polyether used for manufacturing the glass fiber composite material has good fluidity and filling property after being mixed with the polyisocyanate component, is simple to operate, has high finished product qualification rate, and can be used for manufacturing the molding type glass fiber composite material with higher strength requirement.
Detailed Description
The present invention will be further described with reference to the following examples.
All the raw materials used in the examples are commercially available without specific indication.
Example 1
100 kg of combined polyether product is prepared, and weighed polyether polyol A (average functionality is 4-5, and hydroxyl value is 450mgKOH/g) is 37.7 kg, polyether polyol B (functionality is 3, and hydroxyl value is 175mgKOH/g) is 25.1 kg, and polyester polyol C (functionality is 2, and hydroxyl value is 440mgKOH/g) is 20.9 kg. Putting the mixture into a reaction kettle for stirring, then adding 0.8 kg of N, N-dimethylcyclohexylamine, 1.3 kg of N, N-dimethylbenzylamine, 0.3 kg of N, N-dimethyl-propylene-hexahydrotriazine, 0.2 kg of potassium acetate, 0.5 kg of deionized water, 85450.3 kg of Yingchuang Delousai silicone oil B, 12.6 kg of tri (2-chloropropyl) phosphate and 0.5 kg of dyeing-grade nano carbon black, stirring and grinding for 30 minutes to 1 hour, sampling and detecting, and packaging after the mixture is qualified.
The materials and polyphenyl polymethylene polyisocyanate (PAPI) are mixed according to the mass ratio of 1:1.8, are uniformly distributed on the surface of an assembly of a glass fiber and a honeycomb paper core through spraying equipment, and then enter a mold for hot-press molding, so that the polyurethane honeycomb sandwich board can be prepared. The basic properties of the product are as follows:
overall density of the finished product: 155kg/m3
Plane compressive strength: 820KPa
Foam oxygen index: 26.2 percent
Flame retardant grade of the whole workpiece: class A
Example 2
100 kg of combined polyether product is prepared, and weighed polyether polyol A (average functionality is 3-4, and hydroxyl value is 380mgKOH/g) is 32.5 kg, polyether polyol B (functionality is 2, and hydroxyl value is 280mgKOH/g) is 32.5 kg, and polyester polyol C (functionality is 2-3, and hydroxyl value is 175mgKOH/g) is 16.2 kg. Putting the mixture into a reaction kettle for stirring, then adding 0.3 kg of N, N-dimethylcyclohexylamine, 0.4 kg of N, N-dimethylbenzylamine, 0.2 kg of potassium isooctanoate, 1.2 kg of deionized water, 85450.4 kg of Yingchuang Deladmitsai silicone oil B and 16.2 kg of tris (2-chloropropyl) phosphate, stirring for 30 minutes to 1 hour, sampling, detecting, and packaging after the product is qualified.
The materials and diphenylmethane diisocyanate (MDI) are mixed according to the mass ratio of 1:1.2, poured into blocky glass fibers through pouring equipment, and enter a mold for hot press molding, so that the blocky high-strength polyurethane heat insulator can be prepared. The basic properties of the product are as follows:
overall density of the finished product: 143kg/m3
Plane compressive strength: 860KPa
Foam oxygen index: 26.4 percent
Flame retardant grade of the whole workpiece: stage B2
Foam closed cell fraction: more than 90 percent
Thermal conductivity at 20 ℃: 0.24 mW/(m.K)
Comparative example 1
100 kg of combined polyether product is prepared, and weighed polyether polyol A (with the average functionality of 4-5 and the hydroxyl value of 450mgKOH/g) is 40.3 kg, polyether polyol B (with the functionality of 3 and the hydroxyl value of 175mgKOH/g) is 26.9 kg, and polyester polyol C (with the functionality of 2 and the hydroxyl value of 440mgKOH/g) is 22.4 kg. Putting the mixture into a reaction kettle for stirring, then adding 0.9 kg of N, N-dimethylcyclohexylamine, 1.3 kg of N, N-dimethylbenzylamine, 0.3 kg of N, N-dimethyl-propylene-hexahydrotriazine, 0.2 kg of potassium acetate, 0.5 kg of deionized water, 85450.3 kg of Yingchuang Delousai silicone oil B, 6.3 kg of tri (2-chloropropyl) phosphate and 0.5 kg of dyeing-grade nano carbon black, stirring and grinding for 30 minutes to 1 hour, sampling and detecting, and packaging after the mixture is qualified.
The materials and polyphenyl polymethylene polyisocyanate (PAPI) are mixed according to the mass ratio of 1:1.8, are uniformly distributed on the surface of an assembly of a glass fiber and a honeycomb paper core through spraying equipment, and then enter a mold for hot-press molding, so that the polyurethane honeycomb sandwich board can be prepared. The basic properties of the product are as follows:
overall density of the finished product: 146kg/m3
Plane compressive strength: 775KPa
Foam oxygen index: 25.7 percent
Flame retardant grade of the whole workpiece: class B
Due to the fact that the using amount of a flame retardant tri (2-chloropropyl) phosphate is reduced, the oxygen index of the foam is reduced from 26.2% to 25.7, and the integral flame retardant grade of the workpiece cannot reach A-grade flame retardant.
Comparative example 2
100 kg of combined polyether product is prepared, and 24.4 kg of weighed polyether polyol A (average functionality is 3-4, and hydroxyl value is 380mgKOH/g), 40.6 kg of polyether polyol B (functionality is 2, and hydroxyl value is 280mgKOH/g), and 16.2 kg of polyester polyol C (functionality is 2-3, and hydroxyl value is 175 mgKOH/g). Putting the mixture into a reaction kettle for stirring, then adding 0.3 kg of N, N-dimethylcyclohexylamine, 0.4 kg of N, N-dimethylbenzylamine, 0.2 kg of potassium isooctanoate, 1.2 kg of deionized water, 85450.4 kg of Yingchuang Deladmitsai silicone oil B and 16.2 kg of tris (2-chloropropyl) phosphate, stirring for 30 minutes to 1 hour, sampling, detecting, and packaging after the product is qualified.
The materials and diphenylmethane diisocyanate (MDI) are mixed according to the mass ratio of 1:1.2, poured into blocky glass fibers through pouring equipment, and enter a mold for hot press molding, so that the blocky high-strength polyurethane heat insulator can be prepared. The basic properties of the product are as follows:
overall density of the finished product: 141kg/m3
Plane compressive strength: 750KPa
Foam oxygen index: 26.3 percent
Flame retardant grade of the whole workpiece: stage B2
Foam closed cell fraction: 83 percent
Thermal conductivity at 20 ℃: 0.24 mW/(m.K)
Due to the use of too much 2-functionality polyether polyol (from 40 parts to 50 parts), the foam strength properties are significantly reduced and the product curing process is affected, reducing the foam closed cell content to 83%, which is not product specification compliant.
Of course, the foregoing is only a preferred embodiment of the invention and should not be taken as limiting the scope of the embodiments of the invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit and scope of the present invention should be construed as being included in the scope of the present invention.
Claims (10)
1. A conjugate polyether for use in the manufacture of a glass fiber composite, characterized by: the material is prepared from the following raw materials in percentage by mass:
wherein the polyether polyol A is polypropylene oxide polyether polyol with average functionality of 3-6 and molecular weight of 300-1000; the polyether polyol B is polypropylene oxide polyether polyol with average functionality of 2-4 and molecular weight of 500-2000; the polyester polyol C is phthalic anhydride aromatic polyester polyol with average functionality of 2, hydroxyl value of 300-500 mgKOH/g and molecular weight of 200-400.
2. The conjugate polyether for use in the manufacture of a glass fiber composite of claim 1, characterized in that: the foam stabilizer is a Si-C surfactant.
3. The conjugate polyether for use in the manufacture of a glass fiber composite of claim 1, characterized in that: the foaming agent is deionized water.
4. The conjugate polyether for use in the manufacture of a glass fiber composite of claim 1, characterized in that: the catalyst is an organic amine catalyst and/or an organic metal catalyst.
5. The conjugate polyether for use in the manufacture of a glass fiber composite of claim 4, characterized in that: the catalyst is an organic amine catalyst and an organic metal catalyst, wherein the mass ratio of the organic amine catalyst to the organic metal catalyst is 1: 3-3: 1.
6. The conjugate polyether for use in the manufacture of a glass fiber composite of claim 1, characterized in that: the flame retardant is a phosphate ester additive flame retardant.
7. The conjugate polyether for use in the manufacture of a glass fiber composite of claim 6, characterized in that: the flame retardant is a mixture of tris (2-chloropropyl) phosphate and triethyl phosphate, and the mass ratio of the tris (2-chloropropyl) phosphate to the triethyl phosphate is 1: 3-3: 1.
8. A method of preparing the conjugate polyether for use in the manufacture of a glass fiber composite material as claimed in any one of claims 1 to 7, wherein: and uniformly mixing the polyether polyol A, the polyether polyol B and the polyester polyol C, and then adding the catalyst, the foaming agent, the foam stabilizer, the flame retardant and the colorant to uniformly mix to obtain the polyurethane foam.
9. Use of the conjugate polyether as claimed in any one of claims 1 to 7 for the manufacture of a glass fibre composite, wherein: the composite polyether for manufacturing the glass fiber composite material and polyisocyanate are mixed and reacted according to the mass ratio of 1: 1.2-1: 2.2, then are distributed on a base material containing glass fibers, and are molded through a mold, so that the glass fiber composite material is obtained.
10. Use of a conjugate polyether for the manufacture of a glass fiber composite according to claim 9, characterized in that: the polyisocyanate is diphenylmethane diisocyanate and/or polyphenyl methane polyisocyanate.
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| CN201911309903.7A CN110951022A (en) | 2019-12-18 | 2019-12-18 | Conjugate polyether for manufacturing glass fiber composite material and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115058113A (en) * | 2022-07-08 | 2022-09-16 | 重庆欧典实业有限公司 | Fiber-reinforced polyurethane composite material and preparation method and application thereof |
| CN115260741A (en) * | 2022-09-02 | 2022-11-01 | 润德浩远环保科技(北京)有限公司 | Fiber-reinforced polyurethane polymer composite material |
-
2019
- 2019-12-18 CN CN201911309903.7A patent/CN110951022A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115058113A (en) * | 2022-07-08 | 2022-09-16 | 重庆欧典实业有限公司 | Fiber-reinforced polyurethane composite material and preparation method and application thereof |
| CN115260741A (en) * | 2022-09-02 | 2022-11-01 | 润德浩远环保科技(北京)有限公司 | Fiber-reinforced polyurethane polymer composite material |
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Application publication date: 20200403 |