CN103059249A - Preparation method of halogen-free flame-retardant rigid polyurethane foam with zero ozone depletion potential - Google Patents
Preparation method of halogen-free flame-retardant rigid polyurethane foam with zero ozone depletion potential Download PDFInfo
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- CN103059249A CN103059249A CN2013100008761A CN201310000876A CN103059249A CN 103059249 A CN103059249 A CN 103059249A CN 2013100008761 A CN2013100008761 A CN 2013100008761A CN 201310000876 A CN201310000876 A CN 201310000876A CN 103059249 A CN103059249 A CN 103059249A
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Abstract
The invention discloses a preparation method of halogen-free flame-retardant rigid polyurethane foam with zero ozone depletion potential (ODP). The preparation method is characterized in that polymer polyol, foam stabilizer, catalyst, powder foaming agent and flame retardant are stirred electrically to be prepared into a component A, and isocyanate is taken as a component B; when being stirred at high speed, the metered component B is added in a cup filled with the component A and is stirred to be foamed, so that the halogen-free flame-retardant rigid polyurethane foam with zero ODP can be prepared. The invention provides the preparation method of the halogen-free flame-retardant rigid polyurethane foam with zero ODP, which overcomes the defects of low flame retardancy, smokiness, toxicity high ozone depletion potential emission and the like of the conventional polyurethane foam, conforms to the requirements on environmental protection, is simple in process, easy to operate, mild in reaction conditions and easy to control, and is wide in application.
Description
Technical field
The present invention relates to the preparation method of a kind of zero ozone depletion potentiality (ODP) and halogen-free flame-retardant hard polyurethane foam.
Background technology
The multiple excellent properties such as polyurethane rigid foam plastic has that density is little, intensity is high, thermal conductivity is low, water-fast and resistance to acids and bases is good, and have the easy characteristics of the incomparable moulding process of other plastics, so its application almost spreads all over the every profession and trade of national economy.In the preparation process of hard polyurethane foam, foaming is the key of control product density.Polyurethane (PU) rigid foam the eighties in the past always take CFC-11 (monochlorotrifluoromethane) as main auxiliary blowing agent.Because CFC-n is ozone consuming substances (DOS), has higher ODP, global environment is produced destructive influences, be subject to the common concern of international community the eighties, be listed in the chemical of time limit forbidding.
Along with the enhancing of people's environmental protection consciousness, the environmental protection polyurethane foam plastics becomes the focus of various countries' research and development in recent years, and wherein the polyurethane foam of zero odp causes researchist's extensive concern.In PU foaming industry, final what seek is that heat insulating ability, manufacturability, economy aspect can reach simultaneously the level of CFC-n, and meet the whipping agent of the environmental requirement of zero odp.At present, the surrogate of the main low ODP that uses or zero odp mainly comprises for the PU frostproof froth n.: hydrogen fluorohydrocarbon (HFC), alkane, CO
2And water.The whipping agent of hydrogen fluorohydrocarbon (HFC) class needs pressure vessel, because there is larger pressure in Preblend, and needs special schedule of operation; The foam of the whipping agent of alkanes can produce defective, is difficult to be improved and remedy; CO
2Make whipping agent good dimensional stability is only just arranged under HT rate condition; When using water as whipping agent, if it is excessive to control the improper thermal discharge that often can cause, causes product occur to burn core, cracking phenomena and affect quality.Therefore can find out that all there are some defectives in the whipping agent of these liquid state or gaseous state.And this paper adopts the biological whipping agent of a kind of novel zero odp, is pulverulent solids, has replaced above gaseous state or liquid whipping agent.
Compare with flame-retardant polyurethane, only have about 17 without the urethane foam oxygen index of fire-retardant finish, very easily burning in air, a large amount of dense smokes of rear generation on fire cause loss of life and personal injury.At present, the friendly degree of environment requires also more and more higher, and Halogen, efficient, low cigarette, low-poison and combustion-resisting agent have become the important topic of flame retardant area research.The approach that improves flame retardant resistance mainly contains two, and the one, add the compound of the elements such as chloride, bromine, phosphorus, another introduces the atoms such as chlorine, bromine, phosphorus, antimony at polyethers or isocyanic acid ester bond exactly, obtains the structure-type fire retardant material.
The New Phosphorus flame retardant of specialized laboratory of fire retardant material country research and development; with toluene, phenylphosphonothioic dichloride (DCPPS), 1; the 6-hexanediamine is raw material; potassium permanganate is oxygenant, has synthesized fire retardant two (to the amino hexyl-benzoyl of N-) phenyl phosphine oxide (BNBPPO) by four-step reaction.Greatly improved the thermostability of phosphorus flame retardant.The research and development of phosphorus flame retardant and the application present situation in macromolecular material thereof, can find out its development trend be environmental protection, low poison and efficiently, multifunction, and improve its thermostability.Halogen-free flame retardants mainly contains (1) phosphazene compound: a class skeleton is by the inorganic and organic compound of phosphorus and nitrogen-atoms alternative arrangement, carry out nucleophilic substitution reaction by different side groups, can modification and synthetic different macromolecular compound, as new and effective fire retardant, side-chain liquid crystal, specialty elastomer and electronic material etc., (2) Phosphorus annular phosphate DOPO chemical name: 9, the 10-dihydro-9-oxy is mixed-10-phospho hetero phenanthrene-10-oxide compound, outward appearance is white powdery/particle, fusing point 116-119 ℃, 200 ℃ of boiling points (phm), has higher thermostability, oxidation-resistance and good water tolerance, response type and additive flame retardant, (3) tetraphenyl (bisphenol-A) bisphosphate (BDP) there are some researches show that the BDP of use is material modified as fire retardant, although the shock strength of material descends a little, but its oxygen index is up to 30.0%, the UL94 flame retardant properties reaches the V-0 level, evenly heat rate of release (av-HRR) and maximum heat rate of release (pk-HRR) have descended respectively 35.84% and 31.17%, burning time prolongs 18s, intensity of a fire growth indices (FGI) has descended 46.72%, and specific extinction area (SEA) has risen 6.68%.Because the phosphoric acid ester aboundresources is cheap, and is good with the consistency of superpolymer, therefore in organophosphorous fire retardant, be most widely used.
Summary of the invention
This preparation method that a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam are provided, it is low to have overcome existing Polyurethane Rigid Foam Flame Retardance, and thickness is poisonous, and the shortcomings such as high ozone loss potentiality discharging meet environmental requirement.
The present invention is achieved by the following technical solutions:
The preparation method of a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam comprises the steps:
(1) polymer polyatomic alcohol, suds-stabilizing agent, catalyzer, biological powder whipping agent and the fire retardant with metering stirs and prepares the A component, isocyanic ester as the B component;
(2) add the B component of metering in the A component and high-speed stirring makes its foaming, when blending ingredients becomes milky white, stop to stir, leave standstill, sticking to foam till;
(3) put into 60-80 ℃ of baking oven behind the 5-10min, measure its performance behind the slaking 10-12h.
2, described a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam and preparation method thereof is characterized in that the weight part of each raw material is:
Isocyanic ester 34.31-52.28
Polymer polyatomic alcohol 40.33-51.87
Biological powder whipping agent 1.18-1.49
Catalyzer 1.62-2.39
Suds-stabilizing agent 2.16-3.51
Fire retardant 0-16.75
Linking agent 0-1
The preparation method of described a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described isocyanic ester is one or more the mixture in isophorone diisocyanate, poly methylene poly phenyl poly isocyanate, tolylene diisocyanate, '-diphenylmethane diisocyanate, hexamethylene diisocyanate, the dicyclohexyl methane diisocyanate.
The preparation method of described a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described polymer polyatomic alcohol is polyether glycol or polyester polyol, polyvalent alcohol is selected from polytetrahydrofuran polyvalent alcohol, poly-propylene oxide polyvalent alcohol, polyoxyethylene glycol, the mixture of one or more in poly-epsilon-caprolactone glycol, polyethylene glycol adipate glycol, poly-adipate glycol-propylene glycol ester glycol, polybutylene glyool adipate, the poly-carbonic acid hexylene glycol esterdiol.
The preparation method of described a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam is characterized in that: described biological whipping agent is a kind of zero ozone depletion potentiality and efficient Powdered whipping agent K12.
The preparation method of described a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described catalyzer is one or more in stannous octoate, dibutyl tin dilaurate, triethylene diamine, the trolamine.
The preparation method of described a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described suds-stabilizing agent is the organosilicon with Si-C.
The preparation method of described a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described halogen-free flame retardants is to adopt Halogen phosphorus flame retardant methyl-phosphoric acid dimethyl ester and inorganic combustion inhibitor antimonous oxide.
The preparation method of described a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam is characterized in that described linking agent is the polyphenyl polymethylene polyamines.
Beneficial effect of the present invention is:
(1) zero odp halogen-free flame-retardant polyurethane hard bubble composite material can be realized high flame retardant, and low cigarette is nontoxic, the zero odp discharging, and the thing etchant gas produces, and meets environmental requirement;
(2) polyurethane combined material 100% solid content is not cried out any volatile organic matter, environmental friendliness, construction safety in ventilation condition difference ring border is poor;
(3) used polyether glycol, suds-stabilizing agent, catalyzer, whipping agent, fire retardant and isocyanic ester raw material sources are extensive, cheap and easy to get in the experiment;
(4) patent research of the present invention goes out a kind of zero odp halogen-free anti-inflaming polyurethane hard foam, polymer polyatomic alcohol, suds-stabilizing agent, catalyzer, biological powder whipping agent and fire retardant are prepared the A component under electric stirring, then under high-speed stirring, the B component of measuring is joined in the A component, prepare the halogen-free anti-inflaming polyurethane hard foam of excellent performance, this hard polyurethane foam construction is simple, construction costs is low, will be widely used.
Embodiment
Below in conjunction with embodiment the present invention is further described.Content involved in the present invention is not limited only to this five examples.These examples are only listed limited variation with clearer explanation the present invention, do not consist of the restriction of flesh and blood of the present invention.
Embodiment 1
The preparation method of a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam comprises the steps:
(1) polymer polyatomic alcohol, suds-stabilizing agent, catalyzer, biological powder whipping agent and the fire retardant with metering stirs and prepares the A component, isocyanic ester as the B component;
(2) add the B component of metering in the A component and high-speed stirring makes its foaming, when blending ingredients becomes milky white, stop to stir, leave standstill, sticking to foam till;
(3) put into 60 ℃ of baking ovens behind the 5min, measure its performance behind the slaking 12h.
The concrete material that each raw material relates to is: isocyanic ester is isophorone diisocyanate; Polymer polyatomic alcohol is the poly-epsilon-caprolactone glycol; The biological powder whipping agent is sodium lauryl sulphate; Catalyzer is stannous octoate; Suds-stabilizing agent is silicone oil; Fire retardant is methyl-phosphoric acid dimethyl ester; Linking agent is the polyphenyl polymethylene polyamines.
Concrete composition and the weight part of each raw material are:
Isocyanic ester 40.34
Polymer polyatomic alcohol 51.87
Biological powder whipping agent 1.38
Catalyzer 1.90
Suds-stabilizing agent 2.54
Fire retardant 1.96
Linking agent 0-1
Embodiment 2
The preparation method of a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam comprises the steps:
(1) polymer polyatomic alcohol, suds-stabilizing agent, catalyzer, biological powder whipping agent and the fire retardant with metering stirs and prepares the A component, isocyanic ester as the B component;
(2) add the B component of metering in the A component and high-speed stirring makes its foaming, when blending ingredients becomes milky white, stop to stir, leave standstill, sticking to foam till;
(3) put into 60 ℃ of baking ovens behind the 5min, measure its performance behind the slaking 12h.
The concrete material that each raw material relates to is: isocyanic ester is isophorone diisocyanate; Polymer polyatomic alcohol is the poly-epsilon-caprolactone glycol; The biological powder whipping agent is sodium lauryl sulphate; Catalyzer is stannous octoate; Suds-stabilizing agent is silicone oil; Fire retardant is methyl-phosphoric acid dimethyl ester.
The weight part of each raw material is:
Isocyanic ester 39.22
Polymer polyatomic alcohol 50.42
Biological powder whipping agent 1.34
Catalyzer 1.85
Suds-stabilizing agent 2.46
Fire retardant 4.76.
Embodiment 3
The preparation method of a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam, comprise the steps: that (1) stir polymer polyatomic alcohol, suds-stabilizing agent, catalyzer, biological powder whipping agent and the fire retardant of metering to prepare the A component, isocyanic ester as the B component;
(2) add the B component of metering in the A component and high-speed stirring makes its foaming, when blending ingredients becomes milky white, stop to stir, leave standstill, sticking to foam till;
(3) put into 60 ℃ of baking ovens behind the 5min, measure its performance behind the slaking 12h.
The concrete material that each raw material relates to is: isocyanic ester is tolylene diisocyanate; Polymer polyatomic alcohol is the poly-epsilon-caprolactone glycol; The biological powder whipping agent is K12; Catalyzer is stannous octoate; Suds-stabilizing agent is silicone oil; Fire retardant is methyl-phosphoric acid dimethyl ester.
The weight part of each raw material is:
Isocyanic ester 37.43
Polymer polyatomic alcohol 48.13
Biological powder whipping agent 1.28
Catalyzer 1.76
Suds-stabilizing agent 2.35
Fire retardant 9.09.
Embodiment 4
The preparation method of a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam comprises the steps:
(1) polymer polyatomic alcohol, suds-stabilizing agent, catalyzer, biological powder whipping agent and the fire retardant with metering stirs and prepares the A component, isocyanic ester as the B component;
(2) add the B component of metering in the A component and high-speed stirring makes its foaming, when blending ingredients becomes milky white, stop to stir, leave standstill, sticking to foam till;
(3) put into 60 ℃ of baking ovens behind the 5min, measure its performance behind the slaking 12h.
The concrete material that each raw material relates to is: isocyanic ester is tolylene diisocyanate; Polymer polyatomic alcohol is the poly-epsilon-caprolactone glycol; The biological powder whipping agent is K12; Catalyzer is stannous octoate; Suds-stabilizing agent is silicone oil; Fire retardant is methyl-phosphoric acid dimethyl ester.
The weight part of each raw material is:
Isocyanic ester 34.31
Polymer polyatomic alcohol 44.12
Biological powder whipping agent 1.18
Catalyzer 1.62
Suds-stabilizing agent 2.16
Fire retardant 16.75.
Embodiment 5
The preparation method of a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam comprises the steps:
(1) polymer polyatomic alcohol, suds-stabilizing agent, catalyzer, biological powder whipping agent and the fire retardant with metering stirs and prepares the A component, isocyanic ester as the B component;
(2) add the B component of metering in the A component and high-speed stirring makes its foaming, when blending ingredients becomes milky white, stop to stir, leave standstill, sticking to foam till;
(3) put into 60 ℃ of baking ovens behind the 5min, measure its performance behind the slaking 12h.
The concrete material that each raw material relates to is: isocyanic ester is isophorone diisocyanate; Polymer polyatomic alcohol is the poly-epsilon-caprolactone glycol; The biological powder whipping agent is K12; Catalyzer is stannous octoate; Suds-stabilizing agent is silicone oil.
The weight part of each raw material is:
Isocyanic ester 52.28
Polymer polyatomic alcohol 40.33
Biological powder whipping agent 1.49
Catalyzer 2.39
Suds-stabilizing agent 3.51.
Embodiment 6
The preparation method of a kind of zero ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam comprises the steps:
(1) polymer polyatomic alcohol, suds-stabilizing agent, catalyzer, biological powder whipping agent and the fire retardant with metering stirs and prepares the A component, isocyanic ester as the B component;
(2) add the B component of metering in the A component and high-speed stirring makes its foaming, when blending ingredients becomes milky white, stop to stir, leave standstill, sticking to foam till;
(3) put into 60 ℃ of baking ovens behind the 5min, measure its performance behind the slaking 12h.
The concrete material that each raw material relates to is: tolylene diisocyanate; Polymer polyatomic alcohol is the poly-epsilon-caprolactone glycol; The biological powder whipping agent is K12; Catalyzer is stannous octoate; Suds-stabilizing agent is silicone oil; Linking agent is the polyphenyl polymethylene polyamines.
The weight part of each raw material is:
Isocyanic ester 52.28
Polymer polyatomic alcohol 40.33
Biological powder whipping agent 1.49
Catalyzer 2.39
Suds-stabilizing agent 3.51
Linking agent 1.
Above-described embodiment products obtained therefrom is burnt and embodiment 5,6 carries out hardness test, and acquired results is as follows:
Claims (9)
1. the preparation method of zero an ozone depletion potentiality and halogen-free flame-retardant hard polyurethane foam is characterized in that comprising the steps:
(1) polymer polyatomic alcohol, suds-stabilizing agent, catalyzer, biological powder whipping agent and the fire retardant with metering stirs and prepares the A component, isocyanic ester as the B component;
(2) add the B component of metering in the A component and high-speed stirring makes its foaming, when blending ingredients becomes milky white, stop to stir, leave standstill, sticking to foam till;
(3) put into 60-80 ℃ of baking oven behind the 5-10min, measure its performance behind the slaking 10-12h.
2. a kind of zero ozone depletion potentiality according to claim 1 and halogen-free flame-retardant hard polyurethane foam and preparation method thereof it is characterized in that the weight part of each raw material is:
Isocyanic ester 34.31-52.28
Polymer polyatomic alcohol 40.33-51.87
Biological powder whipping agent 1.18-1.49
Catalyzer 1.62-2.39
Suds-stabilizing agent 2.16-3.51
Fire retardant 0-16.75
Linking agent 0-1.
3. the preparation method of a kind of zero ozone depletion potentiality according to claim 1 and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described isocyanic ester is one or more the mixture in isophorone diisocyanate, poly methylene poly phenyl poly isocyanate, tolylene diisocyanate, '-diphenylmethane diisocyanate, hexamethylene diisocyanate, the dicyclohexyl methane diisocyanate.
4. the preparation method of a kind of zero ozone depletion potentiality according to claim 1 and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described polymer polyatomic alcohol is polyether glycol or polyester polyol, polyvalent alcohol is selected from polytetrahydrofuran polyvalent alcohol, poly-propylene oxide polyvalent alcohol, polyoxyethylene glycol, the mixture of one or more in poly-epsilon-caprolactone glycol, polyethylene glycol adipate glycol, poly-adipate glycol-propylene glycol ester glycol, polybutylene glyool adipate, the poly-carbonic acid hexylene glycol esterdiol.
5. the preparation method of a kind of zero ozone depletion potentiality according to claim 1 and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described biological whipping agent is a kind of zero ozone depletion potentiality and efficient Powdered whipping agent K12.
6. the preparation method of a kind of zero ozone depletion potentiality according to claim 1 and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described catalyzer is one or more in stannous octoate, dibutyl tin dilaurate, triethylene diamine, the trolamine.
7. the preparation method of a kind of zero ozone depletion potentiality according to claim 1 and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described suds-stabilizing agent is the organosilicon with Si-C.
8. the preparation method of a kind of zero ozone depletion potentiality according to claim 1 and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described halogen-free flame retardants is to adopt Halogen phosphorus flame retardant methyl-phosphoric acid dimethyl ester and inorganic combustion inhibitor antimonous oxide.
9. the preparation method of a kind of zero ozone depletion potentiality according to claim 1 and halogen-free flame-retardant hard polyurethane foam, it is characterized in that: described linking agent is the polyphenyl polymethylene polyamines.
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Cited By (3)
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| CN104479096A (en) * | 2014-11-19 | 2015-04-01 | 苏州新区佳合塑胶有限公司 | Plastic formula of automobile mattress |
| CN109111558A (en) * | 2018-02-13 | 2019-01-01 | 公安部天津消防研究所 | A kind of low-smoke low-toxicity flame retarded rigid polyurethane foams material and preparation method |
| US11407874B2 (en) | 2019-10-07 | 2022-08-09 | Covestro Llc | Polyol premixes, thermally insulating rigid polyurethane foams and methods for their production |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104479096A (en) * | 2014-11-19 | 2015-04-01 | 苏州新区佳合塑胶有限公司 | Plastic formula of automobile mattress |
| CN109111558A (en) * | 2018-02-13 | 2019-01-01 | 公安部天津消防研究所 | A kind of low-smoke low-toxicity flame retarded rigid polyurethane foams material and preparation method |
| US11407874B2 (en) | 2019-10-07 | 2022-08-09 | Covestro Llc | Polyol premixes, thermally insulating rigid polyurethane foams and methods for their production |
| US11732100B2 (en) | 2019-10-07 | 2023-08-22 | Covestro Llc | Polyol premixes, thermally insulating rigid polyurethane foams and methods for their production |
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Application publication date: 20130424 |