CN110003419B - Pre-gel and preparation method and application thereof - Google Patents
Pre-gel and preparation method and application thereof Download PDFInfo
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- CN110003419B CN110003419B CN201910200977.0A CN201910200977A CN110003419B CN 110003419 B CN110003419 B CN 110003419B CN 201910200977 A CN201910200977 A CN 201910200977A CN 110003419 B CN110003419 B CN 110003419B
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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
- C08G18/4072—Mixtures of compounds of group C08G18/63 with other macromolecular compounds
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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
- C08G18/4833—Polyethers containing oxyethylene units
- C08G18/4837—Polyethers containing oxyethylene units and other oxyalkylene units
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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
- C08G18/63—Block or graft polymers obtained by polymerising compounds having carbon-to-carbon double bonds on to polymers
- C08G18/632—Block or graft polymers obtained by polymerising compounds having carbon-to-carbon double bonds on to polymers onto polyethers
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
- 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)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a pregel and a preparation method and application thereof, wherein the pregel comprises the following components in percentage by mass: 30-40% of sepiolite, 45-55% of water, 2-4% of lauric acid, 6-10% of one or more of alkylphenol polyoxyethylene ether and castor oil polyoxyethylene ether and 3-5% of polymethylene polyphenyl polyisocyanate. Adding sepiolite, water and lauric acid into a container, uniformly mixing at room temperature, adding alkylphenol polyoxyethylene, castor oil polyoxyethylene and polymethylene polyphenyl polyisocyanate, stirring at a high speed of not less than 3500RPM for more than 30min, and standing for 24h to obtain the pre-gel. The pre-gel is used in the formula of the full-water-based low-density flame-retardant flexible polyurethane foam sprayable composition, and can effectively prevent the solid filler from settling.
Description
Technical Field
The invention relates to the field of flexible polyurethane foam, in particular to a solid filler anti-settling technology of a full-water-based low-density flame-retardant flexible polyurethane foam sprayable composition.
Background
Compared with the traditional material, the full water-based soft polyurethane foam spraying system has the advantages that: comprises (1) foaming with water, and zero ODP, and meets the requirement of environmental protection; (2) the foam density is low, the weight is light, the energy is saved, and the cost is saved; (3) the open-cell foam has good moisture resistance and mildew resistance; (4) high production efficiency and the like. Based on the advantages, the full water-based low-density soft polyurethane spray foam can be used as an inner wall heat-insulating and sound-absorbing material in automobile interior and buildings, and can be used as a precision instrument packaging material filling material in transportation, and the like.
With the further upgrade of the national safety and environmental standards, the standard JT/T1095-2016 published in 2016, 12 months, puts more severe requirements on the flame retardance of interior materials of passenger cars in operation, namely: the limiting oxygen index of the material is required to be 28.0%. Patent document CN 102942676 a relates to a full water-based low-density soft polyurethane spray type composite polyether and a preparation method thereof, and CN 108148168A relates to a flame-retardant composite polyether polyol for a passenger car roof, polyurethane foam and a preparation method thereof. On one hand, the technology commonly uses organic halogens and phosphate flame retardants such as tris (1-chloro-ethylpropyl) phosphate (TCPP), tris (1, 3-dichloropropyl) phosphate (TDCP), dimethyl methyl phosphonate (DMMP) and the like, and the halogen-containing material can increase the generation amount of toxic gas and smoke when being combusted; the phosphate flame retardant generally affects the reaction activity of the feed liquid, and can reduce the reaction speed or gradually inactivate the feed liquid; with the increase of the addition amount, the flame retardant also has obvious adverse effect on the environmental protection performance of the foam material. On the other hand, the limit oxygen index of the material disclosed in CN 108148168A is 22% -26%, which does not meet the requirement of the national mandatory standard.
In order to improve the flame retardant property and the environmental protection property of the foam, a certain amount of functional solid filler is often selected to be added into the POLY component, but the problems of material layering, slow reaction speed, low foaming rate and the like of the component are easily caused by directly adding the solid filler.
The anti-settling agent is usually selected to be added for solving the problem of solid settling, but the anti-settling agent in the prior art is not suitable for a formula system of the full-water-based low-density soft polyurethane spraying material. Because of the application requirements of the material, after the solid filler is added, the solid filler has good compatibility and is not easy to settle, the viscosity of the feed liquid is not more than 5000mPa · s at most, and otherwise, the spraying effect is influenced, and even the construction cannot be carried out. In addition, the addition of the anti-settling agent cannot influence the reaction speed and the expansion rate of the material. The anti-settling agent used in the prior art generally increases the viscosity of a feed liquid system or interferes the foaming reaction, and the requirement cannot be met. In the technology described in patent document CN107216707A, the viscosity of the material removing liquid of the anti-settling thickener is greatly increased, and the nonylphenol polyoxyethylene ether used in the technology causes certain harm to the environment, and in the early 2011, Nonylphenol (NP) and Nonylphenol Polyoxyethylene Ether (NPE) are listed as import and export prohibited substances for the first time in toxic chemicals catalog of strict import and export restriction in china issued by ministry of environmental protection and customs administration.
In summary, the prior art mainly has the following defects: the material prepared by the prior art without adding the functional solid filler has flame retardant property and environmental protection property which can not meet the requirements; the direct addition of solid fillers in the prior art formulations is prone to severe delamination and settling; the anti-settling agent used in the prior art has the following problems: greatly increases the viscosity of the system, interferes the foaming reaction, harms the environment and the like.
Disclosure of Invention
The first technical problem to be solved by the present invention is to provide a pregel which is used in the formulation of an all-water based low density flame retardant flexible polyurethane foam sprayable composition and which is effective in preventing the settling of solid fillers.
The second technical problem to be solved by the invention is to provide a preparation method of the pre-gel.
The third technical problem to be solved by the present invention is to provide the use of this pre-gel in a fully water based low density flame retardant flexible polyurethane foam sprayable composition.
In order to solve the first technical problem, the invention provides a pregel which comprises 30-40% of sepiolite, 45-55% of water, 2-4% of lauric acid, 6-10% of one or more of alkylphenol polyoxyethylene ether and castor oil polyoxyethylene ether and 3-5% of polymethylene polyphenyl polyisocyanate by mass.
Suitable alkylphenol ethoxylates such as sec-octylphenol polyethylene (7) ether, sec-octylphenol polyethylene (10) ether, sec-octylphenol polyethylene (15) ether, sec-octylphenol polyethylene (20) ether and the like; suitable castor oil polyoxyethylene ethers are, for example, castor oil polyoxyethylene (20) ether, castor oil polyoxyethylene (30) ether, castor oil polyoxyethylene (40) ether, castor oil polyoxyethylene (60) ether or castor oil polyoxyethylene (80) ether and the like.
To solve the second technical problem, the present invention provides a method for preparing a pre-gel comprising: adding sepiolite, water and lauric acid into a container, uniformly mixing at room temperature, adding alkylphenol polyoxyethylene, castor oil polyoxyethylene and polymethylene polyphenyl polyisocyanate, stirring at a high speed of not less than 3500RPM for more than 30min, and standing for 24h to obtain the pre-gel.
In order to solve the third technical problem, the invention provides an application of a pre-gel in a full water-based low-density flame-retardant flexible polyurethane foam sprayable composition, which is characterized in that the composition contains 10 to 20 mass percent of the pre-gel.
Further, there is provided a fully water-based low density flame retardant flexible polyurethane foam sprayable composition comprising the following components in parts by mass:
the component A comprises: 20 to 30 percent of polyether polyol, 1 to 5 percent of polymer polyol, 20 to 50 percent of solid filler, 8 to 28 percent of water, 0.1 to 5 percent of catalyst, preferably 1 to 3 percent, and 10 to 20 percent of pregel. The component B is general polymethylene polyphenyl polyisocyanate. A. The volume ratio of the component B is 1: 1.
The polyether polyol is preferably one or more of ethylene oxide-propylene oxide copolyether triols with primary hydroxyl content of more than 50% and number average molecular weight of 3000-6500.
The polymer polyol is preferably one or more of styrene-acrylonitrile graft polymer polyols based on ethylene oxide-propylene oxide copolyether triol, the hydroxyl value is 18-30 mgKOH/g, and the solid content is 30-45%.
The solid filler comprises calcium carbonate, talcum powder, ammonium polyphosphate, wollastonite, melamine or aluminum hydroxide and the like, and is not exhaustive.
The catalyst is preferably one or more of Dimethylethanolamine (DMEA), Dimethylaminoethoxyethanol (DMAEE), trimethylhydroxyethylpropylenediamine, N, N, N ' -trimethyl-N ' -hydroxyethyldimethylaminoethyl ether, Tetramethyldipropylenetriamine (TMBPA), N-methyl-N ' -hydroxyethylpiperazine and the like.
Further, a process for preparing a fully water-based flame retardant flexible polyurethane foam sprayable composition comprising the steps of:
the component A comprises: and (2) stirring and mixing polyether polyol, polymer polyol and a catalyst uniformly at 25-40 ℃, then adding water, a solid filler and the pre-gel while stirring, and mixing uniformly.
The component B is directly used.
Compared with the prior art, the invention has the following advantages:
1. the pregel is added into the full water-based low-density flame-retardant soft polyurethane foam spraying composition, and the problems of layering and sedimentation after the solid filler is added are solved under the condition that the viscosity of the system is not greatly increased. Convenient use and no obvious influence on the reaction speed and the foaming ratio of the material. The viscosity of the composition at room temperature is less than 5000mPa & s
2. The preparation method of the pregel is simple.
3. The all-water-based low-density flame-retardant soft polyurethane foam spraying composition provided by the invention is added with the pre-gel, the composition is high in reaction activity and expansion rate, the filler is not easy to settle, the viscosity is suitable for spraying, the composition does not contain an organic solvent, the environment is friendly, and the problems of material layering, slow reaction speed, low foaming rate and the like after the solid filler is added in the prior art are solved.
A pre-gel modified sprayable polyurethane composition containing a functional solid filler, the composition characterized by ease of manufacture; the viscosity is suitable for a spraying process, and the polyurethane foam material prepared by using the composition has higher flame retardant property, environmental protection property and thermal stability.
Detailed Description
The present invention is further illustrated by the following examples, in which the parts are by mass.
Preparation of composition a component: firstly, adding polyether polyol, polymer polyol and a catalyst, and stirring for 15min at 35-40 ℃; adding water, pre-gel and filler while stirring, stirring for 60min at 35-40 ℃, and discharging.
Example 1
Preparation of the pre-gel: 100g of sepiolite, 130g of water and 10g of lauric acid are added into a container, stirred and reacted for 30min at room temperature, 10g of sec-octylphenol polyoxyethylene (15) ether, 18g of castor oil polyoxyethylene (20) ether and 12g of polymethylene polyphenyl polyisocyanate are added, stirred at a high speed for 30min at the rotating speed of 4500RPM or more, and kept stand for 24h, so that the pre-gel is obtained. 10g, 18g of,
EP-551C: ethylene oxide-propylene oxide copolyether triol with the hydroxyl value of 54-58 mgKOH/g; POP 36/28: a polymer polyol having a hydroxyl value of 25 to 29 mgKOH/g.
The component A comprises: EP-551C: 29 parts, POP 36/28: 6 parts of calcium carbonate, 5 parts of melamine, 20 parts of melamine, 25 parts of water, 1 part of dimethylaminoethoxyethanol, 2 parts of N-methyl N' -hydroxyethyl piperazine and 12 parts of pregel. And B component: bayer corporation 44V20L
Example 2
Preparation of the pre-gel: adding 90g of sepiolite, 165g of water and 12g of lauric acid into a container, stirring and reacting at room temperature for 30min, adding 18g of castor oil polyoxyethylene (20) ether and 15g of polymethylene polyphenyl isocyanate, stirring at a high speed of 5000RPM for 30min, and standing for 24h to obtain the pre-gel.
The component A comprises: EP-551C: ethylene oxide-propylene oxide copolyether triol with the hydroxyl value of 54-58 mgKOH/g; CHP-H45: a polymer polyol, CHP-H45, having a hydroxyl value of 19 to 23 mgKOH/g.
The component A comprises: EP-551C: 30 parts, CHP-H45: 3 parts, 2 parts of talcum powder, 20 parts of melamine, 2 parts of ammonium polyphosphate, 20 parts of water, 1 part of dimethylaminoethoxyethanol, 2 parts of N-methyl N' -hydroxyethyl piperazine and 20 parts of pregel.
And B component: bayer corporation 44V20L
Comparative example 1
Comparative example 1 the procedure was the same as in example 1, except that no pregel was added.
The component A comprises: EP 551C: 29 parts, POP 36/28: 6 parts of calcium carbonate, 5 parts of melamine, 20 parts of melamine, 25 parts of water, 1 part of dimethylaminoethoxyethanol and 2 parts of N-methyl N' -hydroxyethyl piperazine.
And B component: bayer corporation 44V20L
Comparative example 2
Comparative example materials the manufacturing process was the same as in the examples, the compositions were different, no pregel was added: POLY component: EP 551C: 29 parts, POP 36/28: 6 parts, 5 parts of calcium carbonate, 20 parts of melamine, 25 parts of water, 1 part of dimethylaminoethoxyethanol and 2 parts of N-methyl N' -hydroxyethyl piperazine, and 5 parts of anti-settling thickening agent and 7 parts of water in a comparative patent CN107216707A are mixed and added into a system.
ISO component: bayer corporation 44V20L
POLY component storage stability test method: 400g of the prepared feed liquid is taken and stored in a 500ml wide-mouth bottle, and the wide-mouth bottle is covered and sealed for storage and is kept for observation.
TABLE 1 comparison of POLY component feed solution parameters
TABLE 2 comparison of foaming parameters and foam Properties
| Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | |
| Rise time/(s) | 3.5 | 4 | 3.5 | 4.5 |
| Curing time/(s) | 9 | 10 | 9 | 12 |
| Density/(kg/m)3) | 10 | 9 | 9 | 18 |
| NP-like inhibiting substance | Does not contain | Does not contain | Does not contain | Comprises |
Claims (7)
1. Use of a pre-gel in a fully water based low density flame retardant flexible polyurethane foam sprayable composition, the pre-gel consisting of in mass fraction: 30-40% of sepiolite, 45-55% of water, 2-4% of lauric acid, 6-10% of one or more of alkylphenol polyoxyethylene ether and castor oil polyoxyethylene ether and 3-5% of polymethylene polyphenyl polyisocyanate; the all-water-based low-density flame-retardant flexible polyurethane foam sprayable composition comprises the following components in parts by mass: the component A comprises: 20-30% of polyether polyol, 1-5% of polymer polyol, 20-50% of solid filler, 8-28% of water, 0.1-5% of catalyst and 10-20% of pre-gel; the component B is polymethylene polyphenyl polyisocyanate; A. the volume ratio of the component B is 1: 1.
2. The use according to claim 1, wherein the alkylphenol ethoxylates are sec-octylphenol polyethylene (7) ether, sec-octylphenol polyethylene (10) ether, sec-octylphenol polyethylene (15) ether or sec-octylphenol polyethylene (20) ether; the castor oil polyoxyethylene ether refers to castor oil polyoxyethylene (20) ether, castor oil polyoxyethylene (30) ether, castor oil polyoxyethylene (40) ether, castor oil polyoxyethylene (60) ether or castor oil polyoxyethylene (80) ether.
3. Use according to claim 1 or 2, the pregel being prepared by a process comprising: adding sepiolite, water and lauric acid into a container, uniformly mixing at room temperature, adding one or more of alkylphenol polyoxyethylene ether and castor oil polyoxyethylene ether and polymethylene polyphenyl polyisocyanate, stirring at a high speed of not less than 3500RPM for more than 30min, and standing for 24h to obtain the pre-gel.
4. The use according to claim 1, wherein the polyether polyol is one or more of ethylene oxide-propylene oxide copolyether triols with a primary hydroxyl group content > 50% and a number average molecular weight of 3000 to 6500.
5. The use of claim 1, wherein the polymer polyol is one or more of styrene-acrylonitrile graft polymer polyols based on ethylene oxide-propylene oxide copolyether triol, and has a hydroxyl value of 18-30 mgKOH/g and a solid content of 30-45%.
6. The use according to claim 1, the solid filler being calcium carbonate, talc, ammonium polyphosphate, wollastonite, melamine or aluminium hydroxide; the catalyst is one or more of Dimethylethanolamine (DMEA), Dimethylaminoethoxyethanol (DMAEE), trimethylhydroxyethylpropylene diamine, N, N, N ' -trimethyl-N ' -hydroxyethyl bisaminoether, Tetramethyldipropylenetriamine (TMBPA) and N-methyl-N ' -hydroxyethyl piperazine.
7. Use according to claim 1, in a process for the preparation of a fully water-based, low density, flame retardant flexible polyurethane foam sprayable composition comprising the steps of: the component A comprises: stirring and mixing polyether polyol, polymer polyol and a catalyst uniformly at 25-40 ℃, then adding water, a solid filler and a pre-gel while stirring, and mixing uniformly; the component B is directly used.
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| CN107936220A (en) * | 2017-12-22 | 2018-04-20 | 上海东大聚氨酯有限公司 | A kind of full water soft flame retardant combined polyether, from its low-density polyurethane continuous slab and preparation method thereof |
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- 2019-03-08 CN CN201910200977.0A patent/CN110003419B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005247892A (en) * | 2004-03-01 | 2005-09-15 | Nippon Paint Co Ltd | Electrodeposition coating composition, method for controlling electrodeposition bath and electrodeposition coating system |
| CN105263982A (en) * | 2013-06-07 | 2016-01-20 | 科思创德国股份公司 | Polyol formulations containing fillers and polyurethanes produced therefrom |
| CN103588953A (en) * | 2013-11-14 | 2014-02-19 | 安徽淮化股份有限公司 | Fire-retardant, low-density and high-resilience soft polyurethane foaming plastic |
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| CN107099187A (en) * | 2017-05-04 | 2017-08-29 | 明光市飞洲新材料有限公司 | A kind of special anti-settling thickener preparation technology of building coating |
| CN107216707A (en) * | 2017-05-04 | 2017-09-29 | 明光市飞洲新材料有限公司 | A kind of special anti-settling thickener of building coating and preparation method thereof |
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