CN103641981A - High fire-retardant conjugate polyether for continuously producing polyurethane board and preparation method of conjugate polyether - Google Patents
High fire-retardant conjugate polyether for continuously producing polyurethane board and preparation method of conjugate polyether Download PDFInfo
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- CN103641981A CN103641981A CN201310714032.3A CN201310714032A CN103641981A CN 103641981 A CN103641981 A CN 103641981A CN 201310714032 A CN201310714032 A CN 201310714032A CN 103641981 A CN103641981 A CN 103641981A
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- 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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
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- 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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- 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
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- 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
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6603—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6614—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6622—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3271
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- 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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- 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
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- 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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- 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
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- 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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- 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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- 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
- C08J2203/184—Binary blends of expanding agents of chemical foaming agent and physical blowing agent, e.g. azodicarbonamide and fluorocarbon
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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
- C08J2375/06—Polyurethanes from polyesters
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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
Abstract
The invention belongs to the field of macromolecules, and particularly relates to high fire-retardant conjugate polyether for continuously producing a polyurethane board. The high fire-retardant conjugate polyether is prepared by the compounding of flame-retardant polyester polyol, polyether polyol, a cross-linking agent, a plurality of catalysts and other raw materials and is applied to the continuous production of a B1-Class high flame-retardant polyurethane board. The preparation method has the advantages that the production efficiency is greatly increased, the comprehensive production cost is decreased, and the problems that a B1-Class high flame-retardant polyurethane board manufactured by a traditional continuous production method is easily cracked, seriously contracted and subjected to secondary foaming can be solved. The board produced through the conjugate polyether prepared by the method disclosed by the invention has fine cells and no crack, and the percentage of contraction is kept below 1.5%; in addition, the board is stable in quality, uniform in density distribution, low in heat conductivity coefficient, high in foam strength and flat in surface. The invention also provides a preparation method of the high fire-retardant conjugate polyether for continuously producing the polyurethane board. The preparation method is simple in process, easy in operation, low in volatilization, out of three wastes (waste gas, waste water and solid waste), stable in product quality, low in production cost and high in production efficiency.
Description
Technical field
The invention belongs to field of polymer technology, be specifically related to a kind of continous way and produce high flame retardant combined polyether and preparation method thereof for polyurethane plate.
Background technology
At present, country is more and more higher to the fire-retardant requirement of the industries such as building board, and continous way production polyurethane plate industry does not also relate to B1 level high flame retardant field.Current workshop for building sheet material, freezer generally require foam by batch process production high flame retardant.Advantage is that facility investment is few, can control the die sinking time, guarantees die sinking after the complete slaking of flame-retardant plate, can not produce the phenomenon of internal cleavage.But shortcoming is quite obvious, first, production efficiency is low; The second, to polyurethane combined material mobility, require quite high; Three, product density skewness, thermal conductivity are high, and quality is unstable.And continous way is produced, efficiency is high, steady quality, and comprehensive production cost is low.But, continous way is produced flame-retardant plate because trimerization reaction is slow at present, be subject to the restriction of continuous lines line length, can not there is the sufficiently long time to carry out trimerization reaction, slaking, so, after rolling off the production line, can form the second time of foaming that foam ftractures, trimerization reaction does not thoroughly cause, cause the phenomenon of the unfairness of plate face, contraction.
Summary of the invention
The object of this invention is to provide a kind of continous way and produce polyurethane plate high flame retardant combined polyether, the sheet material abscess that combined polyether prepared by employing the present invention is produced is fine and smooth, and without cracking, shrinking percentage maintains below 1.5%.The present invention also provides its preparation method, and technique is simple, easy to operate, volatilize low, and without the three wastes, constant product quality, production cost is low, and production efficiency is high.
Continous way of the present invention is produced polyurethane plate high flame retardant combined polyether, by component A and B component, formed, wherein:
Component A is comprised of the raw material of following parts by weight:
B component is polymerization diphenylmethanediisocyanate.
Wherein: described flame retardant polyester polyvalent alcohol A is that functionality 2, molecular weight are 400～-500 polyester polyol;
Described polyether glycol B is the polyether glycol that functionality 4.3, molecular weight are 550～650.
Linking agent is the linking agent that functionality 3, molecular weight are 130～180.Linking agent is preferentially selected trolamine.
Suds-stabilizing agent is non-hydrolysis silicon-carbon class tensio-active agent.Suds-stabilizing agent is preferentially selected B8545 (Ying Chuan group company commercially available prod).
Chemical foaming agent is deionized water.
Catalyzer is the mixture of tertiary amine catalyst and organo-metallic catalyst.Wherein: tertiary amine catalyst is five methyl diethylentriamine, N, N dimethylcyclohexylamine, N, one or more in N dimethyl benzylamine or Hexahydrotriazine are mixed with arbitrary proportion; The preferred five methyl diethylentriamine of tertiary amine catalyst, N, N dimethylcyclohexylamine, N, the mixture of N dimethyl benzylamine and Hexahydrotriazine.Organo-metallic catalyst is that one or both in isocaprylic acid potassium or Potassium ethanoate mix with arbitrary proportion; Organo-metallic catalyst is preferably the mixture of isocaprylic acid potassium and Potassium ethanoate.
Described pneumatogen is HCFC-141b(1, the chloro-1-fluoroethane of 1-bis-).
Described fire retardant is additive flame retardant, three (2-chloropropyl) phosphoric acid ester TCPP.
Described continous way is produced the preparation method of high flame retardant combined polyether for polyurethane plate, comprises the following steps:
(1) component A preparation method: flame retardant polyester polyvalent alcohol A, polyether glycol B, linking agent, stablizer, chemical foaming agent, catalyzer, fire retardant and pneumatogen are mixed successively, and stirring at normal temperature 1～2 hour, obtains component A;
(2) B component is polymerization diphenylmethanediisocyanate, commercial;
(3) component A, B are mixed by the weight proportion of component A: B component=100:185-200, prepare product.
The combined polyether and the isocyanate reaction that adopt the present invention to prepare, continous way is produced and is made high flame retardant foam.Reaching under the fire-retardant prerequisite of B1 level, without cracking phenomena, foam contraction rate is below 1.5%, and density distribution is even, thermal conductivity is low, intensity is high, stable performance, aspect energy-saving and cost-reducing, will play positive urging into effect; Simultaneously production efficiency high, consume energy lowly, greatly reduce comprehensive production cost.
In sum, the present invention has the following advantages:
(1) the present invention adopts the composite high flame retardant combined polyethers that prepare of raw material such as flame retardant polyester polyvalent alcohol, polyether glycol, linking agent and multiple catalysts, is applied to continous way and produces in B1 level high flame-retardant polyurethane sheet material.
(2) the present invention has improved production efficiency greatly, and comprehensive production cost reduces.
(3) A component material is to carry out at normal temperatures, not only save energy but also reduce energy supply equipment and loaded down with trivial details operation.
(4) A component material utilizes HCFC-141b for pneumatogen, keeps foaming properties stable.
(5) overcome the cracking that the B1 of continous way production in the past level flame-retardant plate easily causes, shunk difficult point serious, second time of foaming, the sheet material abscess that combined polyether prepared by employing the present invention is produced is fine and smooth, without cracking, shrinking percentage maintains below 1.5%, and constant product quality, density distribution is even, and thermal conductivity is low, foamy body is high, and plate face is smooth.
(6) preparation method provided by the invention, technique is simple, easy to operate, volatilize low, without the three wastes, constant product quality, production cost is low, and production efficiency is high.The sheet material that combined polyether prepared by employing the present invention is produced, is also to carry out under normal temperature, normal pressure, and technique is simple, easy to operate.
(7) the product indices that the present invention prepares reaches the requirement of GB, adopts after testing the quality index of the B1 level high flame retardant foam that this combined polyether produces, and can reach:
Performance has reached the requirement of GB/T21558-2008 building insulation by standard, GB/T8624-2012 material of construction and the goods combustionproperty B1 level of rigid urethane foam completely.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
Preparation component A, weigh respectively: flame retardant polyester polyvalent alcohol A(2 functionality, molecular weight is 440) 40 kilograms, polyether glycol B(4.3 functionality, molecular weight is 600) 9.3 kilograms, 7.5 kilograms of linking agent trolamines, B85451.4 kilogram (winning wound commercially available), 0.1 kilogram of the sub-ethene triamine of catalyzer pentamethyl-two, N, 0.3 kilogram of N dimethylcyclohexylamine, N, 0.6 kilogram of N dimethyl benzylamine, 0.6 kilogram of Hexahydrotriazine, 1.1 kilograms, isocaprylic acid potassium, 0.8 kilogram of Potassium ethanoate, 1.1 kilograms of deionized waters, HCFC-141b14.2 kilogram, 23 kilograms of three (2-chloropropyl) phosphoric acid ester.By load weighted flame retardant polyester polyvalent alcohol A, polyether glycol B, linking agent, suds-stabilizing agent, chemical foaming agent, catalyzer, pneumatogen and fire retardant, add successively in reactor, stir at normal temperatures 2 hours, taking-up is tested, meet processing parameter, foaming, obtains A component qualified product, takes out barrelling warehouse-in from reactor.
B component is polymerization diphenylmethanediisocyanate, commercial;
Component A, B are mixed by the weight proportion of component A: B component=100:195, prepare continous way and produce high flame retardant combined polyether foam for polyurethane plate, after testing product quality indicator:
Embodiment 2
Preparation component A, weigh respectively: flame retardant polyester polyvalent alcohol A(2 functionality, molecular weight is 400) 50 kilograms, polyether glycol B(4.3 functionality, molecular weight is 550) 7.0 kilograms, 2.3 kilograms of linking agent trolamines, B85452.0 kilogram (winning wound commercially available), 0.5 kilogram of the sub-ethene triamine of catalyzer pentamethyl-two, N, 0.2 kilogram of N dimethylcyclohexylamine, 0.4 kilogram, isocaprylic acid potassium, 0.9 kilogram of Potassium ethanoate, 0.8 kilogram of deionized water, HCFC-141b10.0 kilogram, 15.0 kilograms of three (2-chloropropyl) phosphoric acid ester.By load weighted flame retardant polyester polyvalent alcohol A, polyether glycol B, linking agent, suds-stabilizing agent, chemical foaming agent, catalyzer, pneumatogen and fire retardant, add successively in reactor, stir at normal temperatures 2 hours, taking-up is tested, meet processing parameter, send foam, obtain A component qualified product, from reactor, take out barrelling warehouse-in.
B component is polymerization diphenylmethanediisocyanate, commercial;
Component A, B are mixed by the weight proportion of component A: B component=100:200, prepare continous way and produce high flame retardant combined polyether foam for polyurethane plate, after testing product quality indicator:
Embodiment 3
Preparation component A, weigh respectively: flame retardant polyester polyvalent alcohol A(2 functionality, molecular weight is 500) 43 kilograms, polyether glycol B(4.3 functionality, molecular weight is 650) 15.0 kilograms, 3.2 kilograms of linking agent trolamines, B85451.4 kilogram (winning wound commercially available), 0.1 kilogram of the sub-ethene triamine of catalyzer pentamethyl-two, N, 0.6 kilogram of N dimethyl benzylamine, 0.7 kilogram of Hexahydrotriazine, 1.0 kilograms, isocaprylic acid potassium, 2.5 kilograms of deionized waters, HCFC-141b20.0 kilogram, 30.0 kilograms of three (2-chloropropyl) phosphoric acid ester.By load weighted flame retardant polyester polyvalent alcohol A, polyether glycol B, linking agent, suds-stabilizing agent, chemical foaming agent, catalyzer, pneumatogen and fire retardant, add successively in reactor, stir at normal temperatures 2 hours, taking-up is tested, meet processing parameter, send foam, obtain A component qualified product, from reactor, take out barrelling warehouse-in.
B component is polymerization diphenylmethanediisocyanate, commercial;
Component A, B are mixed by the weight proportion of component A: B component=100:185, prepare continous way and produce high flame retardant combined polyether foam for polyurethane plate, after testing product quality indicator:
Claims (10)
1. continous way is produced a polyurethane plate high flame retardant combined polyether, it is characterized in that: by component A and B component, formed, wherein:
Component A is comprised of the raw material of following parts by weight:
B component is polymerization diphenylmethanediisocyanate;
Wherein: described flame retardant polyester polyvalent alcohol A is the polyester polyol that functionality 2, molecular weight are 400～500;
Described polyether glycol B is the polyether glycol that functionality 4.3, molecular weight are 550～650.
2. continous way according to claim 1 is produced polyurethane plate high flame retardant combined polyether, it is characterized in that: linking agent is the linking agent that functionality 3, molecular weight are 130～180.
3. continous way according to claim 1 is produced polyurethane plate high flame retardant combined polyether, it is characterized in that: suds-stabilizing agent is non-hydrolysis silicon-carbon class tensio-active agent.
4. continous way according to claim 1 is produced polyurethane plate high flame retardant combined polyether, it is characterized in that: chemical foaming agent is deionized water.
5. continous way according to claim 1 is produced polyurethane plate high flame retardant combined polyether, it is characterized in that: catalyzer is the mixture of tertiary amine catalyst and organo-metallic catalyst.
6. continous way according to claim 5 is produced polyurethane plate high flame retardant combined polyether, it is characterized in that: tertiary amine catalyst is five methyl diethylentriamine, N, N dimethylcyclohexylamine, N, one or more in N dimethyl benzylamine or Hexahydrotriazine are mixed with arbitrary proportion.
7. continous way according to claim 5 is produced polyurethane plate high flame retardant combined polyether, it is characterized in that: organo-metallic catalyst is that one or both in isocaprylic acid potassium or Potassium ethanoate mix with arbitrary proportion.
8. continous way according to claim 1 is produced polyurethane plate high flame retardant combined polyether, it is characterized in that: pneumatogen is the chloro-1-fluoroethane of 1,1-bis-.
9. continous way according to claim 1 is produced polyurethane plate high flame retardant combined polyether, it is characterized in that: fire retardant is three (2-chloropropyl) phosphoric acid ester.
10. according to the arbitrary described continous way of claim 1-9, produce a preparation method for high flame retardant combined polyether for polyurethane plate, it is characterized in that: comprise the following steps:
(1) component A preparation method: flame retardant polyester polyvalent alcohol A, polyether glycol B, linking agent, stablizer, chemical foaming agent, catalyzer, fire retardant and pneumatogen are mixed successively, and stirring at normal temperature 1～2 hour, obtains component A;
(2) B component is polymerization diphenylmethanediisocyanate;
(3) component A, B are mixed by the weight proportion of component A: B component=100:185-200, prepare product.
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Cited By (6)
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| CN104193956A (en) * | 2014-09-12 | 2014-12-10 | 上海东方雨虹防水技术有限责任公司 | Rigid polyurethane casting material |
| CN104387549A (en) * | 2014-11-27 | 2015-03-04 | 山东一诺威新材料有限公司 | Combined polyether for flame-retardant bulk rigid polyurethane foams and application method of combined polyether |
| CN104847026A (en) * | 2015-06-03 | 2015-08-19 | 哈尔滨工业大学（威海） | Basalt fiber cloth enhanced polyurethane hard foam composite heat-insulating board and manufacturing method thereof |
| CN105226995A (en) * | 2015-10-21 | 2016-01-06 | 成都九十度工业产品设计有限公司 | A kind of solar energy graphene battery |
| CN105348470A (en) * | 2015-11-25 | 2016-02-24 | 山东一诺威新材料有限公司 | Foamed plastic for low-density and high-flame-retardant continuous slab and preparation method for foamed plastic |
| CN106167540A (en) * | 2016-08-01 | 2016-11-30 | 山东诺威新材料有限公司 | Continuous way produces polyurethane plate high fire-retardance combined polyether and preparation method thereof |
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| CN102532456A (en) * | 2011-12-27 | 2012-07-04 | 山东东大一诺威新材料有限公司 | Environmentally-friendly composition material applied to heat preservation of board and preparation method thereof |
| CN102585148A (en) * | 2011-12-28 | 2012-07-18 | 烟台万华聚氨酯股份有限公司 | Composition for preparing highly fire-resistant polyisocyanurate foam |
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