CN101353422A - Synthetic method of polyether polyatomic alcohol - Google Patents
Synthetic method of polyether polyatomic alcohol Download PDFInfo
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- CN101353422A CN101353422A CNA2008101209201A CN200810120920A CN101353422A CN 101353422 A CN101353422 A CN 101353422A CN A2008101209201 A CNA2008101209201 A CN A2008101209201A CN 200810120920 A CN200810120920 A CN 200810120920A CN 101353422 A CN101353422 A CN 101353422A
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Abstract
The invention discloses a synthetic method of a polyether glycol which belongs to the manufacture technical field of chemical products. The synthetic method of the invention comprises the following steps: sucrose, a compound partly containing active hydrogen, and propylene oxide are taken as raw materials and the polyether glycol is prepared under the effect of a catalyst by the processes of ring opening polymerization, curing, neutralized degasification and dehydrating, etc.; and the synthetic method of the invention is characterized in that: the raw materials also comprise seed oil, and the inventory rating of each component is as follows according to weight percent: 20-25 percent of the sucrose, 2-15 percent of the compound partly containing the active hydrogen, 45-60 percent of the propylene oxide and 5-25 percent of the seed oil, and the total sum of the weight percent of each component is 100 percent; the seed oil can be any one or a mixture of more than one of castor oil, palm oil, soybean oil, cotton seed oil, peanut oil, coconut oil, linseed oil, rapeseed oil, corn, olive oil and sunflower oil, etc. The synthetic method of the invention reasonably chooses the seed oil as raw materials, thus being capable of effectively reducing the usage of the propylene oxide, improving the service performance of the products and reducing the production cost.
Description
Technical field
The present invention relates to a kind of synthetic method of polyether glycol, belong to the manufacturing technology field of Chemicals.
Background technology
Polyether glycol is a main raw material of making rigid urethane foam, it is low that its goods have a thermal conductivity, the characteristics that specific tenacity is high, being widely used in the insulation of buildings and equipment, pipeline, also is the desirable lagging material of building freezer, refrigeration car and boat, refrigerator refrigerator, electric water heater, solar water heater.
The synthetic method of existing cane sugar type rigid-foam polyether polyol mainly is be raw material with sucrose, part active hydrogen compounds, propylene oxide (PO), makes by processes such as ring-opening polymerization, neutralization decolouring, filtration aftertreatments under catalyst action.Though functionality is higher, the combined polyether that is configured to the CFC-11 whipping agent is widely applied in the rigid urethane foam, and the market reflection better.But from CFC-11 whipping agent forbidding till now, China most refrigerator freezer factory has turned to and has used pentamethylene as whipping agent.And the consistency of this polyether glycol and pentamethylene whipping agent is relatively poor, and the combined polyether of configuration is easy to generate muddiness even layering, less stable.
Summary of the invention
It is reasonable to the purpose of this invention is to provide a kind of technology, can effectively improve the product use properties, the synthetic method of the polyether glycol that reduces production costs.
The present invention is a kind of synthetic method of polyether glycol, with sucrose, the part active hydrogen compounds, propylene oxide (PO) is a raw material, under catalyst action by ring-opening polymerization, slaking, the neutralization degassing, operations such as dehydration make, and it is characterized in that also comprising vegetables oil in the raw material, and the charging capacity of each component is respectively by weight percentage: sucrose 20～25%, part active hydrogen compounds 2～15%, propylene oxide 45～60%, vegetables oil 5～25%, the weight percent summation of each component is 100%.
Described vegetables oil can be Viscotrol C, plam oil, soybean oil, Oleum Gossypii semen, peanut oil, Oleum Cocois, linseed oil, rapeseed oil, Semen Maydis oil, sweet oil, the mixture of any one or more of Sunflower Receptacle wet goods.
The described compound that contains reactive hydrogen can be glycol ether, ethylene glycol, propylene glycol, glycerine, sorbyl alcohol, tetramethylolmethane, quadrol, dimethylamine, any one or more mixtures of trolamine etc.
Described catalyzer can be potassium hydroxide, sodium hydroxide, and dimethylamine, any one or more mixtures of quadrol etc., its add-on is 0.2～0.8% of the total charging capacity of raw material.
Described ring-opening polymerization temperature can be 80～130 ℃, and polymerization time is 5～10 hours.
Described curing temperature can be 80～130 ℃, and the curing time is 3～5 hours.
Described dehydration temperaturre can be 105～125 ℃.
The present invention compared with prior art has following outstanding advantage and positively effect:
1, through analysis of experiments, rationally selecting vegetables oil for use is raw material, can effectively reduce the consumption of propylene oxide, has solved in the prior art relatively poorly with pentamethylene whipping agent consistency, is easy to generate muddy even stratified problem.By synthetic plant oil polyether glycol of the present invention, have high functionality, low hydroxyl value, low viscosity, excellent storage stability, and cost is lower.Pentamethylene solubleness can reach more than 35.With the pentamethylene combination material of this polyethers preparation, can under 5 ℃ low temperature, place more than six months, muddiness and demixing phenomenon do not appear.
2, according to vegetables oil be the processing requirement of raw material, through optimization design and repetition test research, rationally determined the processing parameter and the conditions such as temperature, time of operations such as each component proportioning raw materials, catalyst levels, ring-opening polymerization, slaking, dehydration, made the synthetic polyether glycol have high functionality, low hydroxyl value, low viscous characteristics.
3, by synthetic plant oil polyether glycol of the present invention, the production of the combined polyether that is used to hard bubble can be widely used in the insulation of buildings and equipment, pipeline, also is the desirable lagging material of building freezer, refrigeration car and boat, electric water heater, solar water heater etc.Particularly the use of pentamethylene combined polyether on the refrigerator refrigerator with this preparation is extremely extensive.
Embodiment
Synthetic route by existing polyether glycol, suck liquid starting material part active hydrogen compounds, vegetables oil earlier, resorb solid material white sugar, catalyzer, carry out nitrogen replacement 2～3 times, under protection of nitrogen gas, heat up, be evacuated to minimumly, begin to add propylene oxide (PO) and carry out ring-opening polymerization; After adding, propylene oxide (PO) begins slaking, the intact post neutralization degassing of slaking, and processes such as dehydration make polyether glycol.Specific embodiment below in conjunction with processing parameters such as proportioning raw materials, catalyst levels, temperature of reaction, times is further described the present invention.But the present invention is not limited to following embodiment, when practical application, can require and use occasion according to the different performance of polyether glycol, select vegetables oil and proportioning raw materials, initiator and catalyst levels, ring-opening polymerization and processing parameter and conditions such as curing temperature, time among the following embodiment, or processing parameter and condition except that following each embodiment, but all do not limit the scope of the invention in any form.
Embodiment 1: glycol ether 690kg, plam oil 855kg, white sugar 2275kg, potassium hydroxide 35kg, PO5640kg; 105～115 ℃ of ring-opening polymerization temperature, polymerization time 5～10 hours; 110～115 ℃ of curing temperatures, 4 hours curing times; The intact degassing of slaking 15 minutes adds Glacial acetic acid 20kg, and dehydration is extremely qualified, 105～125 ℃ of dehydration temperaturres.
Embodiment 2: propylene glycol 720kg, white sugar 1895kg, dimethylamine 140kg, PO1400kg, first ring-opening polymerization and slaking, 85～95 ℃ of polymerization temperatures, 2～4 hours time; 85～100 ℃ of curing temperatures, 1 hour curing time; The intact back of slaking adds soybean oil 1800kg, dewaters half an hour 105 ℃～110 ℃ of dehydration temperaturres; Continue to add PO2480kg after dehydration finishes and carry out polyreaction and slaking, 105～115 ℃ of polymerization temperatures, 5～10 hours time, 110～115 ℃ of curing temperatures, 3 hours curing times; Outgased 15 minutes, and continued dehydration to qualified, 105～125 ℃ of dehydration temperaturres.
Embodiment 3: glycol ether 1044kg, Oleum Gossypii semen 1340kg, white sugar 1827kg, dimethylamine 44kg, quadrol 35kg, PO4437kg; 105～115 ℃ of ring-opening polymerization temperature, polymerization time 5～10 hours; 110～115 ℃ of curing temperatures, 4 hours curing times; Outgased 15 minutes, and continued dehydration to qualified, 105～125 ℃ of dehydration temperaturres.
Embodiment 4: propylene glycol 150kg, glycol ether 100kg, soybean oil 600kg, white sugar 2100kg, dimethylamine 90kg, PO5400kg; 105～115 ℃ of ring-opening polymerization temperature, polymerization time 5～10 hours; 110～115 ℃ of curing temperatures, 4 hours curing times; Outgased 15 minutes, and continued dehydration to qualified, 105～125 ℃ of dehydration temperaturres.
Embodiment 5: glycerine 300kg, Oleum Gossypii semen 300kg, soybean oil 500kg, white sugar 2100kg, quadrol 50kg, PO5500kg; 105～115 ℃ of ring-opening polymerization temperature, polymerization time 5～10 hours; 110～115 ℃ of curing temperatures, 4 hours curing times; Outgased 15 minutes, and continued dehydration to qualified, 105～125 ℃ of dehydration temperaturres.
Embodiment 6: glycerine 400kg, glycol ether 550kg, Oleum Gossypii semen 950kg, plam oil 950kg, white sugar 1985kg, quadrol 50kg, PO4465kg; 105～115 ℃ of ring-opening polymerization temperature, polymerization time 5～10 hours; 110～115 ℃ of curing temperatures, 4 hours curing times; Outgased 15 minutes, and continued dehydration to qualified, 105～125 ℃ of dehydration temperaturres.
Embodiment 7: glycol ether 895kg, Oleum Gossypii semen 750kg, plam oil 600kg, soybean oil 600kg, white sugar 2185kg, dimethylamine 140kg, PO4430kg; 105～115 ℃ of ring-opening polymerization temperature, polymerization time 5～10 hours; 110～115 ℃ of curing temperatures, 4 hours curing times; Outgased 15 minutes, and continued dehydration to qualified, 105～125 ℃ of dehydration temperaturres.
Embodiment 8: propylene glycol 300kg, Oleum Gossypii semen 500kg, plam oil 500kg, soybean oil 500kg, Viscotrol C 790kg, white sugar 2235kg, dimethylamine 140kg, PO4608kg; 105～115 ℃ of ring-opening polymerization temperature, polymerization time 5～10 hours; 110～115 ℃ of curing temperatures, 4 hours curing times; Outgased 15 minutes, and continued dehydration to qualified, 105～125 ℃ of dehydration temperaturres.
Embodiment 9: propylene glycol 300kg, glycol ether 400kg, glycerine 300kg, Oleum Gossypii semen 450kg, plam oil 450kg, soybean oil 450kg, Viscotrol C 550kg, white sugar 1750kg, dimethylamine 140kg, PO4500kg; 105～115 ℃ of ring-opening polymerization temperature, polymerization time 5～10 hours; 110～115 ℃ of curing temperatures, 4 hours curing times; Outgased 15 minutes, and continued dehydration to qualified, 105～125 ℃ of dehydration temperaturres.
The various embodiments described above are detected, and every performance index are as follows:
Claims (7)
1, a kind of synthetic method of polyether glycol, with sucrose, the part active hydrogen compounds, propylene oxide is a raw material, under catalyst action by ring-opening polymerization, slaking, the neutralization degassing, dehydration procedure makes, and it is characterized in that also comprising vegetables oil in the raw material, and the charging capacity of each component is respectively by weight percentage: sucrose 20～25%, part active hydrogen compounds 2～15%, propylene oxide 45～60%, vegetables oil 5～25%, the weight percent summation of each component is 100%.
2, by the synthetic method of the described a kind of polyether glycol of claim 1, it is characterized in that described vegetables oil is a Viscotrol C, plam oil, soybean oil, Oleum Gossypii semen, peanut oil, Oleum Cocois, linseed oil, rapeseed oil, Semen Maydis oil, sweet oil, the mixture of any one or more of sunflower oil.
3, by the synthetic method of the described a kind of polyether glycol of claim 1, it is characterized in that the described compound that contains reactive hydrogen is a glycol ether, ethylene glycol, propylene glycol, glycerine, sorbyl alcohol, tetramethylolmethane, quadrol, dimethylamine, any one or more mixtures of trolamine.
4, by the synthetic method of the described a kind of polyether glycol of claim 1, it is characterized in that described catalyzer is a potassium hydroxide, sodium hydroxide, dimethylamine, any one or more mixtures of quadrol, its add-on is 0.2～0.8% of the total charging capacity of raw material.
5, by the synthetic method of the described a kind of polyether glycol of claim 1, it is characterized in that described ring-opening polymerization temperature is 80～130 ℃, polymerization time is 5～10 hours.
6, by the synthetic method of the described a kind of polyether glycol of claim 1, it is characterized in that described curing temperature is 80～130 ℃, the curing time is 3～5 hours.
7, described by claim 1, it is characterized in that described dehydration temperaturre is 105～125 ℃.
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| CNA2008101209201A CN101353422A (en) | 2008-09-05 | 2008-09-05 | Synthetic method of polyether polyatomic alcohol |
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| CNA2008101209201A CN101353422A (en) | 2008-09-05 | 2008-09-05 | Synthetic method of polyether polyatomic alcohol |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167808A (en) * | 2011-03-08 | 2011-08-31 | 江苏绿源新材料有限公司 | Method for preparing bio-based polyether glycol from jatropha curcas oil |
| CN102167809A (en) * | 2011-03-08 | 2011-08-31 | 江苏绿源新材料有限公司 | Method for preparing biobased polyether polylol from vegetable oil |
| CN102304223A (en) * | 2011-07-14 | 2012-01-04 | 广州朗腾聚氨酯有限公司 | Plant oil polyether glycol and preparation method thereof |
| CN102532512A (en) * | 2011-12-21 | 2012-07-04 | 山东东大一诺威新材料有限公司 | Method for synthesizing novel polyether polyol |
| CN102558543A (en) * | 2011-12-15 | 2012-07-11 | 福建湄洲湾氯碱工业有限公司 | Synthesis method of plant oil polyether polyol |
| 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 |
| CN104403096A (en) * | 2014-11-27 | 2015-03-11 | 山东一诺威新材料有限公司 | Preparation method of polyether polyol for enhancing intermiscibility of pentane |
| CN104448292A (en) * | 2014-12-09 | 2015-03-25 | 淄博德信联邦化学工业有限公司 | Polyether polyol for high-efficiency strengthening material as well as preparation method of polyether polyol |
| CN105026460A (en) * | 2013-01-15 | 2015-11-04 | 巴斯夫欧洲公司 | Polyols, production and use thereof |
| CN107903388A (en) * | 2017-11-28 | 2018-04-13 | 山东诺威新材料有限公司 | Rigid-foam polyether polyol and preparation method for mining grout material |
| CN108164739A (en) * | 2017-12-27 | 2018-06-15 | 上海东大聚氨酯有限公司 | A kind of fast demoulding polyurethane composition polyethers, polyurethane foam and preparation method thereof |
-
2008
- 2008-09-05 CN CNA2008101209201A patent/CN101353422A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167809A (en) * | 2011-03-08 | 2011-08-31 | 江苏绿源新材料有限公司 | Method for preparing biobased polyether polylol from vegetable oil |
| CN102167808A (en) * | 2011-03-08 | 2011-08-31 | 江苏绿源新材料有限公司 | Method for preparing bio-based polyether glycol from jatropha curcas oil |
| CN102304223A (en) * | 2011-07-14 | 2012-01-04 | 广州朗腾聚氨酯有限公司 | Plant oil polyether glycol and preparation method thereof |
| CN102558543A (en) * | 2011-12-15 | 2012-07-11 | 福建湄洲湾氯碱工业有限公司 | Synthesis method of plant oil polyether polyol |
| CN102532512B (en) * | 2011-12-21 | 2014-05-07 | 山东一诺威新材料有限公司 | Method for synthesizing polyether polyol |
| CN102532512A (en) * | 2011-12-21 | 2012-07-04 | 山东东大一诺威新材料有限公司 | Method for synthesizing novel polyether polyol |
| 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 |
| CN102911354B (en) * | 2012-10-31 | 2014-09-24 | 山东一诺威新材料有限公司 | Preparation method of polyether polyol |
| CN105026460A (en) * | 2013-01-15 | 2015-11-04 | 巴斯夫欧洲公司 | Polyols, production and use thereof |
| CN104403096A (en) * | 2014-11-27 | 2015-03-11 | 山东一诺威新材料有限公司 | Preparation method of polyether polyol for enhancing intermiscibility of pentane |
| CN104448292A (en) * | 2014-12-09 | 2015-03-25 | 淄博德信联邦化学工业有限公司 | Polyether polyol for high-efficiency strengthening material as well as preparation method of polyether polyol |
| CN107903388A (en) * | 2017-11-28 | 2018-04-13 | 山东诺威新材料有限公司 | Rigid-foam polyether polyol and preparation method for mining grout material |
| CN108164739A (en) * | 2017-12-27 | 2018-06-15 | 上海东大聚氨酯有限公司 | A kind of fast demoulding polyurethane composition polyethers, polyurethane foam and preparation method thereof |
| CN108164739B (en) * | 2017-12-27 | 2020-11-24 | 上海东大聚氨酯有限公司 | Polyurethane combined polyether capable of being rapidly demoulded, polyurethane foam and preparation method of polyurethane combined polyether |
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Open date: 20090128 |