CN109438694A - A kind of high activity environment-friendly type rigid-foam polyether and preparation method thereof - Google Patents
A kind of high activity environment-friendly type rigid-foam polyether and preparation method thereof Download PDFInfo
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- CN109438694A CN109438694A CN201811403340.3A CN201811403340A CN109438694A CN 109438694 A CN109438694 A CN 109438694A CN 201811403340 A CN201811403340 A CN 201811403340A CN 109438694 A CN109438694 A CN 109438694A
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- propylene oxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2696—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds characterised by the process or apparatus used
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- Polymers & Plastics (AREA)
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Abstract
The present invention relates to high polymer synthesis technical fields, and in particular to a kind of high activity environment-friendly type rigid-foam polyether and preparation method thereof.A kind of high activity environment-friendly type rigid-foam polyether of the present invention, which is characterized in that be added with following mass component: sucrose: 230-270;Palm oil: 280-320;Amines catalyst: 5-7;Propylene oxide: 380-400;Diethylene glycol (DEG): 70-90.The present invention provides the high activity environment-friendly type rigid-foam polyethers and preparation method thereof that one kind can reduce propylene oxide feed ratio.
Description
Technical field
The present invention relates to high polymer synthesis technical fields, and in particular to a kind of high activity environment-friendly type rigid-foam polyether and its preparation
Method.
Background technique
Polyether polyol (abbreviation polyethers) is by initiator (compound containing active hydrogen group) and ethylene oxide (EO), ring
Ethylene Oxide (PO), epoxy butane (BO) etc. are made through sudden reaction in the presence of a catalyst.Polyethers yield the maximum is with glycerol
(glycerine) is used as initiator and epoxides (usually PO and EO are simultaneously), and by changing the feed way of PO and EO, (mixing adds
Or separately plus), dosage ratio, the charging conditions such as order, produce various general polyether polyol.
With the development of society, the requirement for environmentally friendly machine is continuously improved, which can replace original part
Product.In production process, the feed ratio to propylene oxide is reduced, while reducing the use of catalyst in downstream product production process
Amount.
Based on this, the application is made.
Summary of the invention
The present invention is desirable to provide a kind of high activity environment-friendly type rigid-foam polyether and its system that can reduce propylene oxide feed ratio
Preparation Method, concrete scheme are as follows:
A kind of high activity environment-friendly type rigid-foam polyether is added with following mass component:
Sucrose: 240-280;
Palm oil: 280-320;
Amines catalyst: 5-7;
Propylene oxide: 370-390;
Diethylene glycol (DEG): 60-80.
A kind of preparation method of above-mentioned high activity environment-friendly type rigid-foam polyether, includes the following steps:
(1) 240-280kg sucrose, 280-320kg palm oil are put into, then 28-32kg water carries out nitrogen displacement, displacement is completed
Afterwards after pressure negative pressure to -0.098Mpa, 5-7kg Ammonia catalyst, heating are put into；
(2) pre-reaction, temperature are slowly introducing propylene oxide to 80 DEG C, and when temperature is kept for 80-85 DEG C, pressure is decreased obviously, i.e.,
It is considered as and starts to react, then proceed to be passed through propylene oxide, after which is passed through, temperature is kept for 85-90 DEG C, is opened
Begin to cure；
(3) after curing, it is warming up to 100-110 DEG C, vacuum system is opened, sloughs small point generated in water and reaction process
Son；
(4) after the completion of process (3), temperature is maintained at 100-110 DEG C, is passed through 160-180kg propylene oxide, cures, degassing；
(5) the high activity processing of product puts into 70-90kg diethylene glycol (DEG), and temperature is maintained at 100-110 DEG C, and stirring is dehydrated, pressure
≤ -0.09Mpa, remove the water of reaction generation during this, measure moisture, control range: moisture≤0.1% is passed through after qualified
80-100kg propylene oxide has reached propylene oxide sealing end, further cures, degassing.
A kind of preparation method of above-mentioned high activity environment-friendly type rigid-foam polyether, includes the following steps:
(1) 250kg sucrose, 300kg palm oil are put into, then 30kg water carries out nitrogen displacement, pressure negative pressure after the completion of displacement
After to -0.098Mpa, 6kg Ammonia catalyst, heating are put into；
(2) pre-reaction, temperature are slowly introducing propylene oxide to 80 DEG C, and when temperature is kept for 80-85 DEG C, pressure is decreased obviously, i.e.,
It is considered as and starts to react, then proceed to be passed through propylene oxide, after which is passed through, temperature is kept for 85-90 DEG C, is opened
Begin to cure；
(3) after curing, it is warming up to 100-110 DEG C, vacuum system is opened, sloughs small point generated in water and reaction process
Son；
(4) after the completion of process (3), temperature is maintained at 100-110 DEG C, is passed through 170kg propylene oxide, cures, degassing；
(5) the high activity processing of product puts into 80kg diethylene glycol (DEG), and temperature is maintained at 100-110 DEG C, and stirring is dehydrated, and pressure≤-
0.09Mpa, remove the water of reaction generation during this, measure moisture, control range: moisture≤0.1% is passed through 90kg after qualified
Propylene oxide has reached propylene oxide sealing end, further cures, degassing.
The propylene oxide gross mass that the step (2) is added is 120-130kg.
The invention has the following advantages that
(1) by the use of palm oil, reduce the use for going back Ethylene Oxide, segmentation is passed through propylene oxide, generates during reducing
Small molecule, to reduce consumption of the small molecule to propylene oxide, segmentation reaction, it is ensured that preferable degree of functionality.
(2) present invention uses palm oils, are green material, considerably reduce in polymerization process for epoxy third
The accounting of alkane reduces the consumption of the energy.
(3) a kind of above-mentioned high activity environment-friendly type rigid-foam polyether of the invention improves the application height by activation
The activity of active environment-friendly type rigid-foam polyether.
Specific embodiment
Embodiment 1
(1) 240kg sucrose, 280kg palm oil are put into, then 28kg water carries out nitrogen displacement, pressure negative pressure after the completion of displacement
After to -0.098Mpa, 5kg Ammonia catalyst, heating are put into；
(2) pre-reaction, temperature are slowly introducing propylene oxide to 80 DEG C, and when temperature is kept for 80 DEG C, pressure is decreased obviously, that is, is regarded
To start to react, then proceed to be passed through propylene oxide, after which is passed through, temperature is kept for 85 DEG C, is started ripe
Change；(130kg propylene oxide is added altogether)
(3) after curing, 100 DEG C are warming up to, vacuum system is opened, sloughs the small molecule generated in water and reaction process；
(4) after the completion of process (3), temperature is maintained at 100 DEG C, is passed through 160kg propylene oxide, cures, degassing；
(5) the high activity processing of product puts into 70kg diethylene glycol (DEG), and temperature is maintained at 100 DEG C, and stirring is dehydrated, and pressure≤-
0.09Mpa, remove the water of reaction generation during this, measure moisture, control range: moisture≤0.1% is passed through 80kg after qualified
Propylene oxide has reached propylene oxide sealing end, further cures, degassing.
Testing result: viscosity: 5000mpa s/25 DEG C.
Embodiment 2
(1) 270kg sucrose, 320kg palm oil are put into, then 32kg water carries out nitrogen displacement, pressure negative pressure after the completion of displacement
After to -0.098Mpa, 7kg Ammonia catalyst, heating are put into；
(2) pre-reaction, temperature are slowly introducing propylene oxide to 80 DEG C, and when temperature is kept for 85 DEG C, pressure is decreased obviously, that is, is regarded
To start to react, then proceed to be passed through propylene oxide, after which is passed through, temperature is kept for 90 DEG C, is started ripe
Change；(120kg propylene oxide is added altogether)
(3) after curing, 110 DEG C are warming up to, vacuum system is opened, sloughs the small molecule generated in water and reaction process；
(4) after the completion of process (3), temperature is maintained at 110 DEG C, is passed through 180kg propylene oxide, cures, degassing；
(5) the high activity processing of product puts into 80kg diethylene glycol (DEG), and temperature is maintained at 110 DEG C, and stirring is dehydrated, and pressure≤-
0.09Mpa, remove the water of reaction generation during this, measure moisture, control range: moisture≤0.1% is passed through 90kg after qualified
Propylene oxide has reached propylene oxide sealing end, further cures, degassing.
Testing result: viscosity: 6000mpa s/25 DEG C.
Embodiment 3
(1) 250kg sucrose, 300kg palm oil are put into, then 30kg water carries out nitrogen displacement, pressure negative pressure after the completion of displacement
After to -0.098Mpa, 6kg Ammonia catalyst, heating are put into；
(2) pre-reaction, temperature are slowly introducing propylene oxide to 80 DEG C, and when temperature is kept for 80-85 DEG C, pressure is decreased obviously, i.e.,
It is considered as and starts to react, then proceed to be passed through propylene oxide, after which is passed through, temperature is kept for 88 DEG C, is started
Curing；(130kg propylene oxide is added altogether)
(3) after curing, 106 DEG C are warming up to, vacuum system is opened, sloughs the small molecule generated in water and reaction process；
(4) after the completion of process (3), temperature is maintained at 103 DEG C, is passed through 160kg propylene oxide, cures, degassing；
(5) the high activity processing of product puts into 60kg diethylene glycol (DEG), and temperature is maintained at 107 DEG C, and stirring is dehydrated, and pressure≤-
0.09Mpa, remove the water of reaction generation during this, measure moisture, control range: moisture≤0.1% is passed through 90kg after qualified
Propylene oxide has reached propylene oxide sealing end, further cures, degassing.
Testing result: viscosity: 5500 mpa s/25 DEG C.
Embodiment 4
(1) 280kg sucrose, 300kg palm oil are put into, then 30kg water carries out nitrogen displacement, pressure negative pressure after the completion of displacement
After to -0.098Mpa, 6kg Ammonia catalyst, heating are put into；
(2) pre-reaction, temperature are slowly introducing propylene oxide to 80 DEG C, and when temperature is kept for 80-85 DEG C, pressure is decreased obviously, i.e.,
It is considered as and starts to react, then proceed to be passed through propylene oxide, after which is passed through, temperature is kept for 89 DEG C, is started
Curing；(130kg propylene oxide is added altogether)
(3) after curing, 105 DEG C are warming up to, vacuum system is opened, sloughs the small molecule generated in water and reaction process；
(4) after the completion of process (3), temperature is maintained at 104 DEG C, is passed through 170kg propylene oxide, cures, degassing；
(5) the high activity processing of product puts into 70kg diethylene glycol (DEG), and temperature is maintained at 108 DEG C, and stirring is dehydrated, and pressure≤-
0.09Mpa, remove the water of reaction generation during this, measure moisture, control range: moisture≤0.1% is passed through 90kg after qualified
Propylene oxide has reached propylene oxide sealing end, further cures, degassing.
Testing result: viscosity: 6600 mpa s/25 DEG C.
Above-described embodiment is for the principle of the present invention and its effect to be illustrated, but the present invention is not limited to above-mentioned
Embodiment.Those skilled in the art without departing from the spirit and scope of the present invention, in claims
It is interior, it modifies to above-described embodiment.Therefore protection scope of the present invention, should cover such as claims of the present invention.
Claims (4)
1. a kind of high activity environment-friendly type rigid-foam polyether, which is characterized in that be added with following mass component:
Sucrose: 240-280;
Palm oil: 280-320;
Amines catalyst: 5-7;
Propylene oxide: 370-390;
Diethylene glycol (DEG): 60-80.
2. a kind of preparation method of high activity environment-friendly type rigid-foam polyether as described in claim 1, which is characterized in that including as follows
Step:
(1) 240-280kg sucrose, 280-320kg palm oil are put into, then 28-32kg water carries out nitrogen displacement, displacement is completed
Afterwards after pressure negative pressure to -0.098Mpa, 5-7kg Ammonia catalyst, heating are put into；
(2) pre-reaction, temperature are slowly introducing propylene oxide to 80 DEG C, and when temperature is kept for 80-85 DEG C, pressure is decreased obviously, i.e.,
It is considered as and starts to react, then proceed to be passed through propylene oxide, after which is passed through, temperature is kept for 85-90 DEG C, is opened
Begin to cure；
(3) after curing, it is warming up to 100-110 DEG C, vacuum system is opened, sloughs small point generated in water and reaction process
Son；
(4) after the completion of process (3), temperature is maintained at 100-110 DEG C, is passed through 160-180kg propylene oxide, cures, degassing；
(5) the high activity processing of product puts into 70-90kg diethylene glycol (DEG), and temperature is maintained at 100-110 DEG C, and stirring is dehydrated, pressure
≤ -0.09Mpa, remove the water of reaction generation during this, measure moisture, control range: moisture≤0.1% is passed through after qualified
80-100kg propylene oxide has reached propylene oxide sealing end, further cures, degassing.
3. a kind of preparation method of high activity environment-friendly type rigid-foam polyether as claimed in claim 2, which is characterized in that including as follows
Step:
(1) 250kg sucrose, 300kg palm oil are put into, then 30kg water carries out nitrogen displacement, pressure negative pressure after the completion of displacement
After to -0.098Mpa, 6kg Ammonia catalyst, heating are put into；
(2) pre-reaction, temperature are slowly introducing propylene oxide to 80 DEG C, and when temperature is kept for 80-85 DEG C, pressure is decreased obviously, i.e.,
It is considered as and starts to react, then proceed to be passed through propylene oxide, after which is passed through, temperature is kept for 85-90 DEG C, is opened
Begin to cure；
(3) after curing, it is warming up to 100-110 DEG C, vacuum system is opened, sloughs small point generated in water and reaction process
Son；
(4) after the completion of process (3), temperature is maintained at 100-110 DEG C, is passed through 170kg propylene oxide, cures, degassing；
(5) the high activity processing of product puts into 80kg diethylene glycol (DEG), and temperature is maintained at 100-110 DEG C, and stirring is dehydrated, and pressure≤-
0.09Mpa, remove the water of reaction generation during this, measure moisture, control range: moisture≤0.1% is passed through 90kg after qualified
Propylene oxide has reached propylene oxide sealing end, further cures, degassing.
4. a kind of preparation method of high activity environment-friendly type rigid-foam polyether as described in Claims 2 or 3 any one, feature exist
In: the propylene oxide gross mass that the step (2) is added is 120-130kg.
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| CN201811403340.3A CN109438694A (en) | 2018-11-23 | 2018-11-23 | A kind of high activity environment-friendly type rigid-foam polyether and preparation method thereof |
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| CN201811403340.3A CN109438694A (en) | 2018-11-23 | 2018-11-23 | A kind of high activity environment-friendly type rigid-foam polyether and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US20170088662A1 (en) * | 2007-10-12 | 2017-03-30 | Honeywell International Inc. | Amine catalysts for polyurethane foams |
| CN107151318A (en) * | 2017-06-28 | 2017-09-12 | 山东诺威新材料有限公司 | Sucrose polyethers polyalcohol and preparation method thereof |
| CN108070080A (en) * | 2016-11-18 | 2018-05-25 | 中国石油化工股份有限公司 | A kind of preparation method of urea hard bubble crosslinking agent |
-
2018
- 2018-11-23 CN CN201811403340.3A patent/CN109438694A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170088662A1 (en) * | 2007-10-12 | 2017-03-30 | Honeywell International Inc. | Amine catalysts for polyurethane foams |
| 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 |
| CN108070080A (en) * | 2016-11-18 | 2018-05-25 | 中国石油化工股份有限公司 | A kind of preparation method of urea hard bubble crosslinking agent |
| CN107151318A (en) * | 2017-06-28 | 2017-09-12 | 山东诺威新材料有限公司 | Sucrose polyethers polyalcohol and preparation method thereof |
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Application publication date: 20190308 |