CN104961889A - Preparation method of polyether polyol for rapid demoulding rigid polyurethane foams - Google Patents
Preparation method of polyether polyol for rapid demoulding rigid polyurethane foams Download PDFInfo
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- CN104961889A CN104961889A CN201510320426.XA CN201510320426A CN104961889A CN 104961889 A CN104961889 A CN 104961889A CN 201510320426 A CN201510320426 A CN 201510320426A CN 104961889 A CN104961889 A CN 104961889A
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- polyether glycol
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- fast demoulding
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Abstract
Belonging to the technical field of polyether polyol synthesis, the invention specifically relates to a preparation method of polyether polyol for rapid demoulding rigid polyurethane foams. The method includes: taking solid sorbitol, trimethylolpropane and triethanolamine as the composite initiator, adopting a compounded system of a trimethylamine aqueous solution and DMP-30 as the catalyst, adding oxyalkylene to carry out polymerization and end capping reaction, and finally carrying out demonomerization and drying to obtain the polyether polyol for rapid demoulding rigid polyurethane foams. The polyether polyol prepared by the method provided by the invention has higher flowability, strength and dimensional stability, the rigid foam composite material prepared therefrom and isocyanate react to generate foams with the characteristics of fast curing and short demoulding time, thus greatly improving the production efficiency and saving energy. And compared with existing amidogen ether system composite materials using a special amine initiator, the cost is lower, thereby meeting the high standard requirements of energy saving, consumption reduction, and environmental protection.
Description
Technical field
The invention belongs to polyether glycol synthesis technical field, be specifically related to a kind of preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol.
Background technology
Polyether glycol is one of main raw material of polyurethane industrial, can be used for manufacturing the fields such as automotive trim, medicine equipment, furniture, household electrical appliances, coating, footwear leather.In polyurethane industrial goods, different kinds is for the molecular weight of raw material polyether glycol, functionality, active requirement is different, in polyurethane flexible foam is produced, the functionality of general requirement polyether glycol is 3, molecular weight is even higher 3000, and in order to shorten molding open time in polyurethane moulding flexible foam goods, reduce die temperature save energy, often require the polyether glycol adopting high reactivity and high proportion of primary OH groups, proportion of primary OH groups is more than 70%, the more highly active polyether glycol of manufacturing technique requirent of cold molding, the proportion of primary OH groups of high primary hydroxyl polyether glycol the most frequently used is at present at 75-80%, functionality for hard polyurethane foam production general requirement polyether glycol is greater than 4, molecular weight is at about 400-700, each manufacturer is in order to enhance productivity, save energy, require that production process has shorter open time equally, current polyether glycol aspect generally adopts high functionality, the polyethers system of high hydroxyl value, the amidogen ether that even to arrange in pairs or groups with special amine be initiator, so not only can affect the mobility of foam but also adopt amidogen ether to increase production cost, and rarely have report as adopting in flexible foam production with the patented technology of the high activity polyether of primary hydroxyl end-blocking.
Summary of the invention
The object of this invention is to provide a kind of preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol, obtained polyether glycol has higher activity with primary hydroxyl end-blocking, the hard bubble composite material prepared with it and isocyanate reaction obtain foam there is quick solidifying, degree of crosslinking is high, good stability of the dimension, density calibration is even, good fluidity, the features such as cohesive force is strong, effectively can shorten the open time in molding bubble production process, to enhance productivity save energy, and cost is low compared with existing fast demold system, meet energy-conservation, consumption reduction, the high standard requirement of environmental protection.
The preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol of the present invention is for compound initiator with Neosorb, TriMethylolPropane(TMP), trolamine, the compound system of trimethylamine aqueous solution and DMP-30 is adopted to make catalyzer, add that olefin oxide carries out being polymerized, end capping, fast demoulding use for hard bubble of polyurethane polyether glycol is made in last demonomerization drying.
The mass ratio of described Neosorb, TriMethylolPropane(TMP) and trolamine is 1.5-2.5:1:1.
Described catalyst quality is the 0.5-1% of compound initiator and olefin oxide quality.
Described trimethylamine aqueous solution and the mass ratio of DMP-30 are 3:7-5:5; The mass concentration of trimethylamine aqueous solution is 33-50%, preferred mass concentration 33%.
The preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol of the present invention, step is as follows:
(1) polyreaction: add Neosorb, TriMethylolPropane(TMP), trolamine, trimethylamine aqueous solution, DMP-30 in polymerization reaction kettle, nitrogen replacement, stirring is warming up to 100 DEG C, starts to add propylene oxide and carries out polyreaction, then carry out interior pressure aging reaction;
(2) end capping: temperature rises to 120 DEG C and starts to add oxyethane and carry out end capping, then carries out interior pressure aging reaction;
(3) demonomerization is dry: end capping is aging complete after, carry out vacuumizing demonomerization drying, obtain fast demoulding use for hard bubble of polyurethane polyether glycol.
Polymeric reaction temperature described in step (1) is 105-115 DEG C, and reaction pressure is 0.1-0.3Mpa; The aging reaction time is 1-2h.
Nitrogen replacement number of times described in step (1) is 5-8 time.
End capping temperature described in step (2) is 120-130 DEG C, and reaction pressure is 0.15-0.3Mpa; The aging reaction time is 1-2h.
Oxyethane quality described in step (2) is the 15-25% of propylene oxide and oxyethane total mass.
The demonomerization drying temperature that vacuumizes described in step (3) is 90-110 DEG C, and time of drying is 1-2h, and vacuum degree control is at-0.09 ﹣-0.12Mpa.
The present invention compared with prior art, has following beneficial effect:
The sorbyl alcohol that the present invention adopts molecular structure regular, TriMethylolPropane(TMP), trolamine is as compound initiator, obtained polyether glycol has higher mobility, intensity and dimensional stability, especially oxyethane is adopted to carry out the polyether polyol with high activity of end capping preparation containing primary hydroxyl, effectively can reduce the usage quantity of amines catalyst, reduce smell, the foam that the hard bubble composite material prepared with it and isocyanate reaction generate has quick solidifying, the feature that demould time is short, substantially increase production efficiency, save the energy, and compared with the premixed systems of the amidogen ether system of existing use special amine initiator, there is lower cost, meet energy-conservation, consumption reduction, the high standard requirement of environmental protection.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Agitator is being housed, gauger, heating and temperature controlling device, Neosorb 182g is added in the autoclave of refrigerating unit and pressure transmitter, TriMethylolPropane(TMP) 122g, trolamine 122g, the trimethylamine aqueous solution 2.34g of 33%, DMP-305.48g, nitrogen replacement 5 times, 968gPO drips into reactor when being warming up to 100 DEG C by stirring continuously, temperature of reaction controls at 105-115 DEG C, reaction pressure controls at 0.1-0.3Mpa, reaction no longer changes in rear continuation to pressure presses aging 1h, when being then warming up to 120 DEG C, 171gEO is dripped continuously, temperature of reaction controls at 120-130 DEG C, reaction pressure controls at 0.15-0.3Mpa, reaction to pressure no longer changes the aging 1h of rear continuation, last at 90 DEG C, carry out vacuumizing demonomerization dry reaction 1h under vacuum tightness-0.1Mpa condition and namely obtain fast demoulding use for hard bubble of polyurethane polyether glycol.
Synthesized polyether glycol has following character index:
Outward appearance: colourless to light yellow clear liquid
Hydroxyl value: 410mgKOH/g
Viscosity (25 DEG C): 7049mpa.s
PH：8.93
Functionality: 4.0-4.5
Embodiment 2
Agitator is being housed, gauger, heating and temperature controlling device, Neosorb 182g is added in the autoclave of refrigerating unit and pressure transmitter, TriMethylolPropane(TMP) 91g, trolamine 91g, the trimethylamine aqueous solution 5.54g of 40%, DMP-308.3g, nitrogen replacement 7 times, 816gPO drips into reactor when being warming up to 100 DEG C by stirring continuously, temperature of reaction controls at 105-115 DEG C, reaction pressure controls at 0.1-0.3Mpa, reaction no longer changes in rear continuation to pressure presses aging 1.5h, when being then warming up to 120 DEG C, 204gEO is dripped continuously, temperature of reaction controls at 120-130 DEG C, reaction pressure controls at 0.15-0.3Mpa, reaction to pressure no longer changes the aging 1.5h of rear continuation, last at 100 DEG C, carry out vacuumizing demonomerization dry reaction 2h under vacuum tightness-0.12Mpa condition and namely obtain fast demoulding use for hard bubble of polyurethane polyether glycol.
Synthesized polyether glycol has following character index:
Outward appearance: colourless to light yellow clear liquid
Hydroxyl value: 407mgKOH/g
Viscosity (25 DEG C): 6628mpa.s
PH：9.12
Functionality: 4.0-4.5
Embodiment 3
Agitator is being housed, gauger, heating and temperature controlling device, Neosorb 182g is added in the autoclave of refrigerating unit and pressure transmitter, TriMethylolPropane(TMP) 72g, trolamine 72g, the trimethylamine aqueous solution 5.08g of 50%, DMP-305.08g, nitrogen replacement 8 times, 709gPO drips into reactor when being warming up to 100 DEG C by stirring continuously, temperature of reaction controls at 105-115 DEG C, reaction pressure controls at 0.1-0.3Mpa, reaction no longer changes in rear continuation to pressure presses aging 1h, when being then warming up to 120 DEG C, 236gEO is dripped continuously, temperature of reaction controls at 120-130 DEG C, reaction pressure controls at 0.15-0.3Mpa, reaction to pressure no longer changes the aging 2h of rear continuation, last at 110 DEG C, carry out vacuumizing demonomerization dry reaction 1.5h under vacuum tightness-0.10Mpa condition and namely obtain fast demoulding use for hard bubble of polyurethane polyether glycol.
Synthesized polyether glycol has following character index:
Outward appearance: colourless to light yellow clear liquid
Hydroxyl value: 415mgKOH/g
Viscosity (25 DEG C): 7210mpa.s
PH：9.33
Functionality: 4.0-4.5
Polyether glycol prepared by embodiment 1,2 and 3 carries out hard polyurethane foam Performance Detection, and with containing the amidogen ether YD-401P (functionality 4 that is initiator with special amine, hydroxyl value 380) the hard polyurethane foams prepared of fast lift-off system contrast, comparing result is in table 1.
The performance comparison of hard polyurethane foam prepared by table 1
As can be seen from Table 1, hard polyurethane foam good fluidity prepared by the fast demoulding use for hard bubble of polyurethane polyether glycol prepared by the present invention, compressive strength is high, and low-temperature shrink deformation rate is little, and especially open time obviously shortens.Shorter open time can effectively improve in hard polyurethane foam production process production efficiency, save energy, compared with the system of hard bubbling of existing use amidogen ether, can effectively shorten open time about 15-20% under same processing condition, cost is low, has higher cost performance.
Claims (10)
1. the preparation method of a fast demoulding use for hard bubble of polyurethane polyether glycol, it is characterized in that with Neosorb, TriMethylolPropane(TMP), trolamine for compound initiator, the compound system of trimethylamine aqueous solution and DMP-30 is adopted to make catalyzer, add that olefin oxide carries out being polymerized, end capping, fast demoulding use for hard bubble of polyurethane polyether glycol is made in last demonomerization drying.
2. the preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol according to claim 1, is characterized in that the mass ratio of described Neosorb, TriMethylolPropane(TMP) and trolamine is 1.5-2.5:1:1.
3. the preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol according to claim 1, is characterized in that described catalyst quality is the 0.5-1% of compound initiator and olefin oxide quality.
4. the preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol according to claim 1, it is characterized in that the mass ratio of described trimethylamine aqueous solution and DMP-30 is 3:7-5:5, the mass concentration of trimethylamine aqueous solution is 33-50%.
5., according to the preparation method of the arbitrary described fast demoulding use for hard bubble of polyurethane polyether glycol of claim 1-4, it is characterized in that step is as follows:
(1) polyreaction: add Neosorb, TriMethylolPropane(TMP), trolamine, trimethylamine aqueous solution, DMP-30 in polymerization reaction kettle, nitrogen replacement, stirring is warming up to 100 DEG C, starts to add propylene oxide and carries out polyreaction, then carry out interior pressure aging reaction;
(2) end capping: temperature rises to 120 DEG C and starts to add oxyethane and carry out end capping, then carries out interior pressure aging reaction;
(3) demonomerization is dry: end capping is aging complete after, carry out vacuumizing demonomerization drying, obtain fast demoulding use for hard bubble of polyurethane polyether glycol.
6. the preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol according to claim 5, it is characterized in that the polymeric reaction temperature described in step (1) is 105-115 DEG C, reaction pressure is 0.1-0.3Mpa; The aging reaction time is 1-2h.
7. the preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol according to claim 5, is characterized in that the nitrogen replacement number of times described in step (1) is 5-8 time.
8. the preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol according to claim 5, it is characterized in that the end capping temperature described in step (2) is 120-130 DEG C, reaction pressure is 0.15-0.3Mpa; The aging reaction time is 1-2h.
9. the preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol according to claim 5, is characterized in that the oxyethane quality described in step (2) is the 15-25% of propylene oxide and oxyethane total mass.
10. the preparation method of fast demoulding use for hard bubble of polyurethane polyether glycol according to claim 5, it is characterized in that the demonomerization drying temperature that vacuumizes described in step (3) is 90-110 DEG C, time of drying is 1-2h, and vacuum degree control is at-0.09 ﹣-0.12Mpa.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4451588A (en) * | 1983-07-26 | 1984-05-29 | Texaco Inc. | High load bearing polyurethane foams made from mixed initiator polyether polyols |
| CN102453253A (en) * | 2010-10-21 | 2012-05-16 | 中国石油化工集团公司 | Method for preparing higher primary hydroxyl polyether polyalcohol |
| CN102781996A (en) * | 2010-03-02 | 2012-11-14 | 巴斯夫欧洲公司 | Method for producing polyurethane hard foam materials |
| CN102911354A (en) * | 2012-10-31 | 2013-02-06 | 山东东大一诺威新材料有限公司 | Preparation method of polyether polyol |
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- 2015-06-11 CN CN201510320426.XA patent/CN104961889A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4451588A (en) * | 1983-07-26 | 1984-05-29 | Texaco Inc. | High load bearing polyurethane foams made from mixed initiator polyether polyols |
| CN102781996A (en) * | 2010-03-02 | 2012-11-14 | 巴斯夫欧洲公司 | Method for producing polyurethane hard foam materials |
| CN102453253A (en) * | 2010-10-21 | 2012-05-16 | 中国石油化工集团公司 | Method for preparing higher primary hydroxyl polyether polyalcohol |
| CN102911354A (en) * | 2012-10-31 | 2013-02-06 | 山东东大一诺威新材料有限公司 | Preparation method of polyether polyol |
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