CN105315449A - Polyether polyol used for low-density gaseousness and slow-resilience foam, preparation method of polyether polyol and slow-resilience foam and preparation method thereof - Google Patents
Polyether polyol used for low-density gaseousness and slow-resilience foam, preparation method of polyether polyol and slow-resilience foam and preparation method thereof Download PDFInfo
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Abstract
The invention relates to polyether polyol used for low-density gaseousness and slow-resilience foam, a preparation method of the polyether polyol and the slow-resilience foam and a preparation method thereof and belongs to the technical field of organic macromolecule synthesis. A polyhydric alcohol compound with small molecular weight serves as an initiator of the polyether polyol, and an end group is copolymer of epoxypropane with the end capped with ethylene oxide and ethylene oxide monomer; the preparation method of the polyether polyol comprises the steps of making the polyhydric alcohol compound with the small molecular weight and a catalyst be subjected to a reaction in a pressure-proof reaction kettle, then sequentially adding polymerization monomer, water, phosphoric acid and magnesium silicate for reaction, and obtaining the polyether polyol; the slow-resilience foam is prepared from a component A and a component B, wherein the component A comprises the polyether polyol, a composite catalyst, silicone oil and a foaming agent, and the component B is modified MDI; the preparation method of the slow-resilience foam comprises the steps of mixing the component A with the component B uniformly, then pouring the mixture into a mold for curing, and obtaining the slow-resilience foam. The slow-resilience foam prepared through the preparation method has the advantages of being low in density, good in gaseousness property and free of shrinkage, and the preparation method of the slow-resilience foam is simple and easy to operate.
Description
Technical field
The present invention relates to a kind of low density flatulence low resilience urethane foam resilient foam polyether glycol and preparation method thereof and low resilience urethane foam resilient foam and preparation method thereof, belong to organic polymer synthesis technical field.
Background technology
Low resilience urethane foam resilient foam is also known as viscoelastic foam or memory foam, there is the functions such as shape memory, energy-absorbing, sound-absorbing, shock-absorbing, often by as absorbing body, acoustic(al)absorbent, shock absorber and be widely used in the fields such as furniture, bedclothes, auto parts machinery, sports equipment, medicine equipment due to it.During using low resilience urethane foam resilient foam as cushion material and mat, pressure distribution evenly, the changing of the relative positions of sense of fatigue and bottom surface can be reduced.The raw material preparing low resilience urethane foam resilient foam at present mainly coordinates with some high activity polyethers and small molecules slow rebound polyether, the low resilience urethane foam resilient foam closed pore of preparation is serious, shrinkability is very strong, therefore the special pore-creating agent of some low resilience must be added in formula, and the density of the low resilience urethane foam resilient foam of preparation is relatively high, is approximately 70-80kg/m
3, feel is also relatively coarse, does not have moistening comfort, and the low resilience urethane foam resilient foam prepared thus more and more can not meet the requirement of market to low density, high-comfort low resilience urethane foam resilient foam.Therefore, be necessary that exploitation one has high-comfort and flatulence, and there is the low density low resilience urethane foam resilient foam polyether glycol of certain perforate performance, break away from the dependence to pore-creating agent simultaneously.
Summary of the invention
The object of this invention is to provide a kind of low density flatulence low resilience urethane foam resilient foam polyether glycol, have that reactive behavior is high, foaming slaking fireballing feature, the present invention provides preparation method simultaneously; The low resilience urethane foam resilient foam that the present invention also provides a kind of low density flatulence low resilience urethane foam resilient foam polyether glycol to prepare, have that density is low, flatulence but do not shrink, feature that hand feel and drape is good, provide its preparation method simultaneously.
Low density flatulence low resilience urethane foam resilient foam polyether glycol of the present invention is with small-molecular-weight polyol compound for initiator, and end group is ethylene oxide-capped propylene oxide and the multipolymer of oxirane monomers, and hydroxyl value is 32-44mgKOH/g; Wherein, polymerization single polymerization monomer oxypropylene accounts for 5-30wt%, and oxyethane accounts for 70-95wt%.
Described small-molecular-weight polyol compound is one or more in ethylene glycol, propylene glycol, neopentyl glycol, glycerol, TriMethylolPropane(TMP) (TMP), tetramethylolmethane, sorbyl alcohol.
The preparation method of described low density flatulence low resilience urethane foam resilient foam polyether glycol, comprises the following steps:
(1) in withstand voltage reactor, add small-molecular-weight polyol compound and the catalyzer of metering, meet oxygen level≤50ppm after nitrogen replacement 3-5 time, be then warming up to 100-120 DEG C, be evacuated to-0.092MPa, dehydration reaction 5-8h;
(2) passing ratio adjusting mixer adds propylene oxide and oxirane monomers continuously in withstand voltage reactor, at 120-130 DEG C, carry out polyreaction, continues reaction 2h after reinforced; Then vacuumize to remove unreacted residual monomer, after being cooled to 80-90 DEG C, be transferred to aftertreatment still;
(3) in aftertreatment still, pure water and phosphoric acid stirring reaction 0.5-1h is added, and then add Magnesium Silicate q-agent continuation stirring 0.5-1h, dehydration 5-10h is vacuumized after being warming up to 100-110 DEG C, circulating filtration to solution is water white transparency shape, obtains the polyether glycol for low density flatulence low resilience urethane foam resilient foam.
Wherein, preferred technical scheme is as follows:
In step (1), catalyzer is one or more in KOH, NaOH, sodium methylate, and its consumption accounts for the 0.2-0.4% of the bullet polyether glycol quality obtained in step (3).
In step (3), pure water consumption accounts for the 2.0-5.0% of polyether glycol quality; Phosphoric acid consumption accounts for the 0.4-0.8% of polyether glycol quality; Magnesium Silicate q-agent consumption accounts for the 0.1-0.2% of polyether glycol quality.
Low resilience urethane foam resilient foam prepared by low density flatulence low resilience urethane foam resilient foam polyether glycol of the present invention, is made up of component A and B component, wherein:
With weight parts, component A is made up of following raw material:
Wherein: the gross weight number of polyether glycol A, polyether glycol B, polyether glycol C tri-kinds of raw materials is 100 parts;
Described polyether glycol A is with small-molecular-weight polyol compound for initiator, and end group is ethylene oxide-capped propylene oxide and the multipolymer of oxirane monomers, and hydroxyl value is 32-44mgKOH/g; Wherein, polymerization single polymerization monomer oxypropylene accounts for 5-30wt%, and oxyethane accounts for 70-95wt%; Small-molecular-weight polyol compound is one or more in ethylene glycol, propylene glycol, neopentyl glycol, glycerol, TriMethylolPropane(TMP) (TMP), tetramethylolmethane, sorbyl alcohol;
Described polyether glycol B is polymer polyatomic alcohol, and model is GPOP-30, and manufacturer is Shanghai Gaoqiao petrochemical corporation (complex);
Described polyether glycol C is polyethers 1030;
Described composite catalyst is the mixture of DMEA, catalysts for polyurethanes A-1, catalysts for polyurethanes A-33 and catalysts for polyurethanes A-300, and manufacturer is US Air gas chemical company;
Described silicone oil be model be respectively in L-580 and B8002 one or both;
Described whipping agent is H
2one or both in O, HCFC-141B, methylene dichloride (MC);
B component:
Modification MDI.
Described modification MDI is DG5412, modification MDI8019 or modification MDI2412.Wherein, the manufacturer of DG5412 is Shandong Inov Polyurethane Co., Ltd., and the manufacturer of modification MDI8019 is Wan Hua chemical groups company limited, and the manufacturer of modification MDI2412 is Huntsman Polyurethanes company limited.
The preparation method of low resilience urethane foam resilient foam of the present invention, comprises the following steps:
(1) polyether glycol A, polyether glycol B, polyether glycol C, composite catalyst, silicone oil, whipping agent are fully mixed, obtain component A;
(2) component A and B component are at room temperature mixed, be then poured into slaking 3-5min in mould, obtain low resilience urethane foam resilient foam.
Wherein:
Isocyanate index in described step (2) when component A and B component mixing controls within the scope of 60-90.
Beneficial effect of the present invention is as follows:
Low density flatulence low resilience urethane foam resilient foam polyether glycol of the present invention has that reactive behavior is high, foaming slaking fireballing feature, and be particularly useful for making low density slow-recovery sponge foam, its preparation method is simple, easy to operate; Have that density is low, flatulence good with low resilience urethane foam resilient foam prepared by low density flatulence low resilience urethane foam resilient foam polyether glycol but do not shrink, press and fall into residual low and that low-temperature flexibility is good feature, its preparation method simple and feasible.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Low density flatulence low resilience urethane foam resilient foam polyether glycol take TriMethylolPropane(TMP) as initiator, and end group is ethylene oxide-capped propylene oxide and the multipolymer of oxirane monomers.Wherein, polymerization single polymerization monomer oxypropylene accounts for 30wt%, and oxyethane accounts for 70wt%.
Preparation method is as follows:
(1) in withstand voltage reactor, add the KOH of TMP and 10g of 134g, nitrogen replacement 3 times, after measured, oxygen level is 45ppm, is warming up to 110 DEG C, is evacuated to-0.092MPa, dehydration reaction 5h;
(2) passing ratio adjusting mixer adds 1460g propylene oxide and 3406g oxirane monomers continuously in withstand voltage reactor, at 120 DEG C, carry out polyreaction, continues reaction 2h after reinforced; Then be evacuated to-0.092MPa, remove unreacted residual monomer, after being cooled to 90 DEG C, be transferred to aftertreatment still;
(3) in aftertreatment still, add 150g pure water and 20g phosphoric acid stirring reaction 1h, and then add 5g Magnesium Silicate q-agent continuation stirring 0.5h, vacuumize dehydration 6h after being warming up to 110 DEG C, circulating filtration to solution is water white transparency shape, obtains low density flatulence low resilience urethane foam resilient foam polyether glycol.
After testing, the OHv=33.82mgKOH/g of the low density flatulence low resilience urethane foam resilient foam polyether glycol obtained.
The low density flatulence low resilience urethane foam resilient foam polyether glycol obtained with the present embodiment prepares low resilience urethane foam resilient foam, fills a prescription as follows:
With weight parts, component A is made up of following raw material:
B component:
DG5412。
Preparation method is as follows:
Component A and B component are at room temperature mixed according to the ratio that weight ratio is 100:45.5, be then poured into slaking 4min in mould, obtain low resilience urethane foam resilient foam after die sinking, specific performance Testing index is in table 1.
Embodiment 2
Low density flatulence low resilience urethane foam resilient foam polyether glycol is that end group is ethylene oxide-capped propylene oxide and the multipolymer of oxirane monomers with glycerol and neopentyl glycol for initiator.Wherein, polymerization single polymerization monomer oxypropylene accounts for 15wt%, and oxyethane accounts for 85wt%.
Preparation method is as follows:
(1) in withstand voltage reactor, add the NaOH of the glycerol of 61.33g, the neopentyl glycol of 34.67g and 13.2g, nitrogen replacement 4 times, after measured, oxygen level is 40ppm, is warming up to 110 DEG C, is evacuated to-0.092MPa, dehydration reaction 7h;
(2) passing ratio adjusting mixer adds 646g propylene oxide and 3658g oxirane monomers continuously in withstand voltage reactor, at 120 DEG C, carry out polyreaction, continues reaction 2h after reinforced; Then be evacuated to-0.092MPa, remove unreacted residual monomer, after being cooled to 85 DEG C, be transferred to aftertreatment still;
(3) in aftertreatment still, add 176g pure water and 26.5g phosphoric acid stirring reaction 1h, and then add 6.6g Magnesium Silicate q-agent continuation stirring 0.5h, vacuumize dehydration 8h after being warming up to 110 DEG C, circulating filtration to solution is water white transparency shape, obtains low density flatulence low resilience urethane foam resilient foam polyether glycol.
After testing, the OHv=34.02mgKOH/g of the low density flatulence low resilience urethane foam resilient foam polyether glycol obtained.
The low density flatulence low resilience urethane foam resilient foam polyether glycol obtained with the present embodiment prepares low resilience urethane foam resilient foam, fills a prescription as follows:
With weight parts, component A is made up of following raw material:
B component:
Modification MDI8019.
Preparation method is as follows:
Component A and B component are at room temperature mixed according to the ratio that weight ratio is 100:43.2, be then poured into slaking 5min in mould, obtain low resilience urethane foam resilient foam after die sinking, specific performance Testing index is in table 1.
Embodiment 3
Low density flatulence low resilience urethane foam resilient foam polyether glycol is that end group is ethylene oxide-capped propylene oxide and the multipolymer of oxirane monomers with glycerol and sorbyl alcohol for initiator.Wherein, polymerization single polymerization monomer oxypropylene accounts for 5wt%, and oxyethane accounts for 95wt%.
Preparation method is as follows:
(1) in withstand voltage reactor, add the NaOH of the glycerol of 59.28g, the sorbyl alcohol of 23.45g and 16.4g, nitrogen replacement 5 times, after measured, oxygen level is 28ppm, is warming up to 110 DEG C, is evacuated to-0.092MPa, dehydration reaction 8h;
(2) passing ratio adjusting mixer adds 230.3g propylene oxide and 4367g oxirane monomers continuously in withstand voltage reactor, at 120 DEG C, carry out polyreaction, continues reaction 2h after reinforced; Then be evacuated to-0.092MPa, remove unreacted residual monomer, after being cooled to 80 DEG C, be transferred to aftertreatment still;
(3) in aftertreatment still, add 187g pure water and 33g phosphoric acid stirring reaction 1h, and then add 8.4g Magnesium Silicate q-agent continuation stirring 0.5h, vacuumize dehydration 8h after being warming up to 110 DEG C, circulating filtration to solution is water white transparency shape, obtains low density flatulence low resilience urethane foam resilient foam polyether glycol.
After testing, the OHv=41.95mgKOH/g of the low density flatulence low resilience urethane foam resilient foam polyether glycol obtained.
The low density flatulence low resilience urethane foam resilient foam polyether glycol obtained with the present embodiment prepares low resilience urethane foam resilient foam, fills a prescription as follows:
With weight parts, component A is made up of following raw material:
B component:
Modification MDI2412.
Preparation method is as follows:
Component A and B component are at room temperature mixed according to the ratio that weight ratio is 100:41, be then poured into slaking 4min in mould, obtain low resilience urethane foam resilient foam after die sinking, specific performance Testing index is in table 1.
Table 1 low resilience urethane foam resilient foam Performance Detection index
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Isocyanate index | 80 | 90 | 70 |
| Foam core density (Kg/m 3) | 42 | 46 | 40 |
| Shrinkability | Flatulence but do not shrink | Flatulence but do not shrink | Flatulence but do not shrink |
| Second-order transition temperature (DEG C) | -65/-3 | -67/-5 | -70/-7 |
| Tensile strength (KPa) | 99 | 110 | 95 |
| Rebound degree (%) | 9.0 | 8.2 | 9.2 |
| Resilience time (s) | 4 | 6 | 5 |
| Compression set (%) | 2.5 | 3.0 | 2.3 |
Note: low resilience urethane foam resilient foam has two second-order transition temperatures, and second-order transition temperature is lower, the low-temperature flexibility of foam is better.
Claims (10)
1. a low density flatulence low resilience urethane foam resilient foam polyether glycol, is characterized in that: be with small-molecular-weight polyol compound for initiator, and end group is ethylene oxide-capped propylene oxide and the multipolymer of oxirane monomers, and hydroxyl value is 32-44mgKOH/g; Wherein, polymerization single polymerization monomer oxypropylene accounts for 5-30wt%, and oxyethane accounts for 70-95wt%;
Described small-molecular-weight polyol compound is one or more in ethylene glycol, propylene glycol, neopentyl glycol, glycerol, TriMethylolPropane(TMP), tetramethylolmethane, sorbyl alcohol.
2. a preparation method for low density flatulence low resilience urethane foam resilient foam polyether glycol according to claim 1, is characterized in that: comprise the following steps:
(1) in withstand voltage reactor, add small-molecular-weight polyol compound and the catalyzer of metering, meet oxygen level≤50ppm after nitrogen replacement 3-5 time, be then warming up to 100-120 DEG C, be evacuated to-0.092MPa, dehydration reaction 5-8h;
(2) passing ratio adjusting mixer adds propylene oxide and oxirane monomers continuously in withstand voltage reactor, at 120-130 DEG C, carry out polyreaction, continues reaction 2h after reinforced; Then vacuumize to remove unreacted residual monomer, after being cooled to 80-90 DEG C, be transferred to aftertreatment still;
(3) in aftertreatment still, pure water and phosphoric acid stirring reaction 0.5-1h is added, and then add Magnesium Silicate q-agent continuation stirring 0.5-1h, dehydration 5-10h is vacuumized after being warming up to 100-110 DEG C, circulating filtration to solution is water white transparency shape, obtains the polyether glycol for low density flatulence low resilience urethane foam resilient foam.
3. the preparation method of low density flatulence low resilience urethane foam resilient foam polyether glycol according to claim 2, it is characterized in that: in step (1), catalyzer is one or more in KOH, NaOH, sodium methylate, and its consumption accounts for the 0.2-0.4% of the polyether glycol quality obtained in step (3).
4. the preparation method of low density flatulence low resilience urethane foam resilient foam polyether glycol according to claim 2, is characterized in that: in step (3), pure water consumption accounts for the 2.0-5.0% of the polyether glycol quality obtained; Phosphoric acid consumption accounts for the 0.4-0.8% of the polyether glycol quality obtained; Magnesium Silicate q-agent consumption accounts for the 0.1-0.2% of the polyether glycol quality obtained.
5., with a low resilience urethane foam resilient foam prepared by low density flatulence low resilience urethane foam resilient foam polyether glycol according to claim 1, it is characterized in that: be made up of component A and B component, wherein:
With weight parts, component A is made up of following raw material:
Wherein, the gross weight number of polyether glycol A, polyether glycol B, polyether glycol C tri-kinds of raw materials is 100 parts;
Described polyether glycol A is with small-molecular-weight polyol compound for initiator, and end group is ethylene oxide-capped propylene oxide and the multipolymer of oxirane monomers, and hydroxyl value is 32-44mgKOH/g; Wherein, polymerization single polymerization monomer oxypropylene accounts for 5-30wt%, and oxyethane accounts for 70-95wt%; Small-molecular-weight polyol compound is one or more in ethylene glycol, propylene glycol, neopentyl glycol, glycerol, TriMethylolPropane(TMP), tetramethylolmethane, sorbyl alcohol;
Described polyether glycol B is polymer polyatomic alcohol, and model is GPOP-30;
Described polyether glycol C is polyethers 1030;
B component:
Modification MDI.
6. low resilience urethane foam resilient foam according to claim 5, is characterized in that: described composite catalyst is the mixture of DMEA, catalysts for polyurethanes A-1, catalysts for polyurethanes A-33 and catalysts for polyurethanes A-300.
7. low resilience urethane foam resilient foam according to claim 5, is characterized in that: silicone oil be the trade mark be respectively in L-580 and B8002 one or both; Whipping agent is H
2one or both in O, HCFC-141B, methylene dichloride.
8. low resilience urethane foam resilient foam according to claim 5, is characterized in that: modification MDI is DG5412, modification MDI8019 or modification MDI2412.
9. a preparation method for the arbitrary described low resilience urethane foam resilient foam of claim 5-8, is characterized in that: comprise the following steps:
(1) polyether glycol A, polymer polyatomic alcohol B, polyether glycol C, composite catalyst, silicone oil, whipping agent are fully mixed, obtain component A;
(2) component A and B component are at room temperature mixed, be then poured into slaking 3-5min in mould, obtain low resilience urethane foam resilient foam.
10. the preparation method of low resilience urethane foam resilient foam according to claim 9, is characterized in that: the isocyanate index in step (2) when component A and B component mixing controls within the scope of 60-90.
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