CN109824873A - It is a kind of for full water foamed polyester polyol and preparation method thereof - Google Patents
It is a kind of for full water foamed polyester polyol and preparation method thereof Download PDFInfo
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- CN109824873A CN109824873A CN201910071857.5A CN201910071857A CN109824873A CN 109824873 A CN109824873 A CN 109824873A CN 201910071857 A CN201910071857 A CN 201910071857A CN 109824873 A CN109824873 A CN 109824873A
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Abstract
The present invention provides a kind of for full water foamed polyester polyol and preparation method thereof, which includes: binary acid or acid anhydrides, fatty acid, polyalcohol and catalyst.It is above-mentioned to have the characteristics that low viscosity, high functionality for full water foamed polyester polyol, greatly improve the full water foamed white material viscosity height for embodying and depositing, the shortcomings that poor fluidity, it is above-mentioned to be used in full water foamed polyester polyol use process, foam bubble is fine and closely woven, good stability of the dimension effectively improves the anti-flammability and cementability of foam.
Description
Technical field
The invention belongs to polyester polyol technical field more particularly to it is a kind of for full water foamed polyester polyol and
Preparation method.
Background technique
Hard polyurethane foams have extremely low thermal coefficient, have with multiple material with good adhesive strength, form work
Skill is simple, is widely used in refrigerator, hot duct, Cold Chain Logistics, external wall of house etc..Polyurethane foam is by polyethers or polyester
What polyalcohol, foaming agent, surfactant and isocyanates generated under the effect of the catalyst.Polyester polyol is that synthesis is poly-
One of the important source material of urethane hard bubble, polyester polyol are to pass through polycondensation by dicarboxylic acids and dihydric alcohol or polyalcohol etc. mostly
What reaction obtained.According to the selection of different material, the polyester polyol of different properties can be produced, is widely used in various
In hard polyurethane foam foaming system.
And the inflammable and explosive foaming agent such as pentamethylene is in transport to storing, convenience for construction etc. has very big office
It is sex-limited.Therefore the use of physical blowing agent receives serious resistance.Full water foamed main reacted using water and isocyanates is given birth to
At carbon dioxide gas foam, be foaming technique initially use in polyurethane foam process engineering.Water is most honest and clean
Valence, most environmentally friendly chemical reaction shaping foam agent, and have effect of crucial importance in polyurethane foam technique always.Working as
Under preceding Environmental Protection Situation, full water foamed because of environmental-friendly (zero odp, low GWP), use is safe, and use cost is lower, is regarded
For the mainstream technology in the following hard polyurethane foam field.And the polyester requirement viscosity for being used for full water foamed system is small, good fluidity,
The high-functionality polyester polyol viscosity of domestic production at present is generally higher, and especially low temperature flow is very poor and Quan Shuifa
The compatibility of foam system becomes a urgent problem to be solved.Furthermore existing using the full water foamed of full polyethers, foam it is fire-retardant
Performance and surface cementability are insufficient.Therefore, it is a imperative for full water foamed polyester polyol to research and develop.
Summary of the invention
Being designed to provide for the embodiment of the present invention is a kind of for full water foamed polyester polyol and preparation method thereof,
It aims to solve the problem that in existing polyester polyol use process, the foam anti-flammability caused by large viscosity, poor fluidity and viscous
The problem of connecing property difference.
The embodiments of the present invention are implemented as follows, a kind of for full water foamed polyester polyol, including includes: binary
Acid or acid anhydrides, fatty acid, polyalcohol and catalyst.
It is above-mentioned to be used for full water foamed polyester polyol, have the characteristics that low viscosity, high functionality, greatly improves
The shortcomings that full water foamed white material viscosity deposited that embodies is high, poor fluidity, it is above-mentioned to be used for full water foamed polyester polyol
Cheng Zhong, foam bubble is fine and closely woven, good stability of the dimension, effectively improves the anti-flammability and cementability of foam.
Further, the binary acid is 120~140 parts, and the fatty acid is 40~120 parts, and the polyalcohol is
330~620 parts, the catalyst is 0.5~2 part.
Further, the binary acid includes phthalic anhydride, and the polyalcohol includes diethylene glycol, poly- second two
The mixture of one or more of alcohol, glycerine or sorbierite.
Further, polyethylene glycol described in the polyalcohol be 200~240 parts, the diethylene glycol be 80~
140 parts, the sorbierite is 0~160 part, and the glycerine is 50~80 parts.
Further, the fatty acid includes the mixture of one or more of oleic acid, soybean oil or palm oil.
Further, the catalyst includes butyl titanate, stannous octoate, Dibutyltin oxide, tin dilaurate two
The mixture of one or more of butyl tin oxide.
The another object of the embodiment of the present invention be to provide it is a kind of for full water foamed PEPA preparation method,
Include:
Raw material is sent into reaction kettle, nitrogen and heat temperature raising are passed through, the raw material includes binary acid or acid anhydrides, fat
Acid, polyalcohol and catalyst；
Start to stir after raw material melting, and when the temperature in the reaction kettle reaches the first preset temperature, root
The reaction kettle, which is controlled, according to first preset temperature carries out heated at constant temperature；
When determining the condenser top temperature drop in the reaction kettle down to the second preset temperature, being passed through for nitrogen is closed,
And vacuumize process is carried out to the reaction kettle；
When determining within the scope of the current vacuum level arrival predetermined vacuum degree in the reaction kettle, according to described current
Reaction kettle described in vacuum degree control carries out Isobarically Control, and controls the reaction kettle and persistently heated with preset temperature range,
Until taking out polyester polyol when determining that moisture is evaporated in the raw material.
Above-mentioned to be used for full water foamed PEPA preparation method, preparation step is simple, prepares stable reaction, and make
The polyester polyol obtained has the characteristics that low viscosity, high functionality, greatly improves the full water foamed white material viscosity for embodying and depositing
The shortcomings that height, poor fluidity.
Further, described after determining the step of moisture is evaporated in the raw material, the method is also wrapped
It includes:
Judge whether the polyester polyol in the reaction kettle meets discharging condition；
If it is not, then issuing warning note.
It further, include multiple judgement parameters in the discharging condition, it is described to judge parameter for the polyester polyols
The hydroxyl value of molecular weight of polyesters in alcohol whether reach 280~300mgKOH/g, the polyester polyol acid value whether≤
Whether 3mgKOH/g, the polyester polyol viscosity are 800~1500mPaS, whether the moisture of the polyester polyol is small
In 0.1% or the polyester polyol degree of functionality whether >=3.
Further, first preset temperature is 210 DEG C~230 DEG C, and second preset temperature is to 60~70
DEG C, the predetermined vacuum degree range is 0.09~0.095MPa, and the preset temperature range is 220~230 DEG C.
Detailed description of the invention
Fig. 1 is the flow chart for full water foamed PEPA preparation method that sixth embodiment of the invention provides；
The present invention that the following detailed description will be further explained with reference to the above drawings.
Specific embodiment
For the ease of more fully understanding the present invention, the present invention is carried out below in conjunction with related embodiment attached drawing further
It explains on ground.The embodiment of the present invention is given in attached drawing, but the present invention is not limited in above-mentioned preferred embodiment.On the contrary, mentioning
Purpose for these embodiments be in order to make disclosure of the invention face more sufficiently.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
Centainly refer to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be any
One or more embodiment or examples in can be combined in any suitable manner.
In order to illustrate technical solutions according to the invention, the following is a description of specific embodiments
Embodiment one
First embodiment of the invention provides a kind of for full water foamed polyester polyol, comprising: binary acid or acid anhydrides,
Fatty acid, polyalcohol and catalyst, the polyester polyol have the characteristics that low viscosity, high functionality, greatly improve complete
The shortcomings that white material viscosity that Water blown embodiment is deposited is high, poor fluidity, it is above-mentioned to be used for full water foamed polyester polyol use process
In, foam bubble is fine and closely woven, good stability of the dimension, effectively improves the anti-flammability and cementability of foam.
Embodiment two
Second embodiment of the invention provides a kind of for full water foamed polyester polyol, comprising: binary acid or acid anhydrides,
Fatty acid, polyalcohol and catalyst, the binary acid include phthalic anhydride, and the polyalcohol includes diethylene glycol, poly- second
The mixture of one or more of glycol, glycerine or sorbierite, the fatty acid include oleic acid, soybean oil or palm oil
One or more of mixture, the catalyst includes butyl titanate, stannous octoate, Dibutyltin oxide, two laurels
The mixture of one or more of sour Dibutyltin oxide.
In the present embodiment, compared with prior art, the polyester polyol in the present embodiment has low viscosity, high functionality
The characteristics of, the shortcomings that it is high greatly to improve the full water foamed white material viscosity deposited of embodying, poor fluidity.It is complete in existing mainstream
Under Water blown formula, the pure and mild polyether polyol mix and match of polyester polyols in the present embodiment is used, and foam bubble is fine and closely woven, ruler
Very little stability is good, also improves the anti-flammability and cementability of foam to a certain extent.Polyester polyol in the present embodiment is opposite
For the polyether polyol that full water foamed system is widely used at present, there are certain cost advantage, sexual valence with higher
Than.The product is not related to hazardous chemical in raw material selection, and technique is relatively easy, securely and reliably.
Embodiment three
Third embodiment of the invention provides a kind of for full water foamed polyester polyol, comprising: binary acid or acid anhydrides,
Fatty acid, polyalcohol and catalyst, the binary acid include phthalic anhydride, and the polyalcohol includes diethylene glycol, poly- second
The mixture of one or more of glycol, glycerine or sorbierite, the fatty acid include oleic acid, soybean oil or palm oil
One or more of mixture, the catalyst includes butyl titanate, stannous octoate, Dibutyltin oxide, two laurels
The mixture of one or more of sour Dibutyltin oxide.
Specifically, including 120~140 parts of phthalic anhydride in the binary acid in the present embodiment；
It include 110~120 parts of soybean oil in the fatty acid；
In the polyalcohol include polyethylene glycol 200~240 part, 80~100 parts of diethylene glycol, sorbierite 140~160
Part, 70~80 parts of glycerine；
The catalyst uses 1.5 parts of Dibutyltin oxide；
In the present embodiment, compared with prior art, the polyester polyol in the present embodiment has low viscosity, high functionality
The characteristics of, the shortcomings that it is high greatly to improve the full water foamed white material viscosity deposited of embodying, poor fluidity.It is complete in existing mainstream
Under Water blown formula, the pure and mild polyether polyol mix and match of polyester polyols in the present embodiment is used, and foam bubble is fine and closely woven, ruler
Very little stability is good, also improves the anti-flammability and cementability of foam to a certain extent.Polyester polyol in the present embodiment is opposite
For the polyether polyol that full water foamed system is widely used at present, there are certain cost advantage, sexual valence with higher
Than.The product is not related to hazardous chemical in raw material selection, and technique is relatively easy, securely and reliably.
Example IV
Third embodiment of the invention provides a kind of for full water foamed polyester polyol, including phthalic anhydride 130
Part, the oxidation of 115 parts of soybean oil, 220 parts of polyethylene glycol, 90 parts of diethylene glycol, 150 parts of sorbierite, 75 parts of glycerine, dibutyl
1.5 parts of tin；
In the present embodiment, compared with prior art, the polyester polyol in the present embodiment has low viscosity, high functionality
The characteristics of, the shortcomings that it is high greatly to improve the full water foamed white material viscosity deposited of embodying, poor fluidity.It is complete in existing mainstream
Under Water blown formula, the pure and mild polyether polyol mix and match of polyester polyols in the present embodiment is used, and foam bubble is fine and closely woven, ruler
Very little stability is good, also improves the anti-flammability and cementability of foam to a certain extent.Polyester polyol in the present embodiment is opposite
For the polyether polyol that full water foamed system is widely used at present, there are certain cost advantage, sexual valence with higher
Than.The product is not related to hazardous chemical in raw material selection, and technique is relatively easy, securely and reliably.
Embodiment five
Fifth embodiment of the invention provides a kind of for full water foamed polyester polyol, including phthalic anhydride 140
Part, the oxidation of 120 parts of soybean oil, 240 parts of polyethylene glycol, 100 parts of diethylene glycol, 160 parts of sorbierite, 80 parts of glycerine, dibutyl
1.5 parts of tin；
In the present embodiment, compared with prior art, the polyester polyol in the present embodiment has low viscosity, high functionality
The characteristics of, the shortcomings that it is high greatly to improve the full water foamed white material viscosity deposited of embodying, poor fluidity.It is complete in existing mainstream
Under Water blown formula, the pure and mild polyether polyol mix and match of polyester polyols in the present embodiment is used, and foam bubble is fine and closely woven, ruler
Very little stability is good, also improves the anti-flammability and cementability of foam to a certain extent.Polyester polyol in the present embodiment is opposite
For the polyether polyol that full water foamed system is widely used at present, there are certain cost advantage, sexual valence with higher
Than.The product is not related to hazardous chemical in raw material selection, and technique is relatively easy, securely and reliably.
Embodiment six
Referring to Fig. 1, being sixth embodiment of the invention offer for full water foamed PEPA preparation method
Flow chart, raw material include: 120~140 parts of phthalic anhydride, and 110~120 parts of soybean oil, polyethylene glycol 200~240 part,
80~100 parts of diethylene glycol, 140~160 parts of sorbierite, 70~80 parts of glycerine, 1.5 parts of catalyst (Dibutyltin oxide)；
Specifically, comprising steps of
Raw material is sent into reaction kettle by step S11, is passed through nitrogen and heat temperature raising；
Step S21 starts to stir after raw material melting, and presets when the temperature in the reaction kettle reaches first
When temperature, the reaction kettle is controlled according to first preset temperature and carries out heated at constant temperature；
Wherein, first preset temperature is 220 DEG C, in the step, when reaction temperature reaches 170 DEG C, and each raw material institute
The moisture content contained is distilled out of, and continues to be heated to 220 DEG C, keeps the temperature 3 hours, during which described in reaction kettle inner condenser top temperature
It controls within 103 DEG C；
Step S31 closes nitrogen when determining the condenser top temperature drop in the reaction kettle down to the second preset temperature
Gas is passed through, and carries out vacuumize process to the reaction kettle；
Wherein, temperature range locating for second preset temperature is 60~70 DEG C, sufficiently reacts and steams to raw material in kettle
Most of moisture content when condenser top temperature drops to 60~70 DEG C, closes being passed through for nitrogen, and starts slowly to vacuumize；
Step S41, when determining within the scope of the current vacuum level arrival predetermined vacuum degree in the reaction kettle, according to
The current vacuum level controls the reaction kettle and carries out Isobarically Control；
Step S51 is controlled the reaction kettle and is persistently heated with preset temperature range, until determining the raw material
In water and reaction process in the water that generates drained completely, polycondensation reaction is completed, and indices meet design afterwards after tested
It is required that taking out polyester polyol；
Wherein, the predetermined vacuum degree range is 0.09~0.095MPa, the preset temperature range is 220~230
DEG C, in the step, until vacuum degree reaches 0.09~0.095MPa, and keep the vacuum degree 1 hour, it is warm in present invention kettle
Degree should be maintained between 220~230 DEG C, be fully drawn out the moisture content in raw material.Raw material contracts during vacuumizing
Poly- reaction molecular amount increases quickly, the indices of polyester is constantly detected in the period, index can stop in computer capacity
Only vacuumize.It can discharge when polyester polyol is cooled to 100 DEG C or so canned.
Preferably, show that the polyester polyol color is clear pale yellow color through operation；Hydroxyl value 292mgKOH/g, acid value
1.2mgKOH/g, at 25 DEG C, viscosity is 1500PaS, 0.1% or less moisture.Comply fully with polyester under full water foamed system
The index request of polyalcohol.
Application for present case has chosen the formula of some maturations in full water foamed field, by polyester produced by the invention
Polyalcohol is substituted into the formula (polyether polyol instead of 70%).
Table one: the application formula of full water foamed polyester polyol case 3
Survey the specific time parameter of foaming process are as follows: rise time 7~9 seconds；The wire drawing time 13~14 seconds；When surface drying
Between 45~55 seconds.
Above-mentioned to be used for full water foamed PEPA preparation method, preparation step is simple, prepares stable reaction, and make
The polyester polyol obtained compared with prior art, has the characteristics that low viscosity, high functionality, greatly improves full water foamed
The shortcomings that white material viscosity that embodiment is deposited is high, poor fluidity.It is poly- in the present embodiment under the full water foamed formula of existing mainstream
Ester polyol and polyether polyol mix and match use, and foam bubble is fine and closely woven, and good stability of the dimension is also promoted to a certain extent
The anti-flammability and cementability of foam.Polyester polyol in the present embodiment is widely used at present relative to full water foamed system
Polyether polyol for, have certain cost advantage, cost performance with higher.The product is not related in raw material selection
Hazardous chemical, technique is relatively easy, securely and reliably.
Embodiment seven
Seventh embodiment of the invention provides a kind of for full water foamed PEPA preparation method, and raw material includes: neighbour
200~230 parts of phthalate anhydride, 60~70 parts of oleic acid, 350~400 parts of polyethylene glycol, 220~250 parts of diethylene glycol, the third three
80~90 parts of alcohol, 0.5 part of catalyst (Dibutyltin oxide)；
The preparation step of fourth embodiment of the invention is identical as the preparation step of Fig. 1 in embodiment three, obtains this through operation
Polyester polyol color is transparent yellowish；Hydroxyl value 285mgKOH/g, acid value 1.0mgKOH/g are in 25 DEG C of viscosity
1050mPaS, 0.1% or less moisture.Comply fully with the index request of polyester polyol under full water foamed system.
Application for present case has chosen the formula of full water foamed field maturation, and the formula is identical as in case 1,
Polyester polyol produced by the invention is substituted into the formula (polyether polyol of replacement 70%):
| Classification | Title | Mass fraction |
| Polyester polyol | 4 products obtained therefrom of embodiment | 70 |
| Polyether polyol | YD-8310 | 30 |
| Catalyst | A33+ cyclohexylamine | 1+1 |
| Silicone oil | AK-8805 | 2 |
| Foaming agent | Water | 4 |
| Isocyanates | 120 | |
| It is other | Glycerine | 1 |
Table two: the application formula of full water foamed polyester polyol example 4
Survey the specific time parameter of foaming process are as follows: rise time 7~9 seconds；The wire drawing time 13~14 seconds；When surface drying
Between 45~55 seconds.
Above-mentioned to be used for full water foamed PEPA preparation method, preparation step is simple, prepares stable reaction, and make
The polyester polyol obtained compared with prior art, has the characteristics that low viscosity, high functionality, greatly improves full water foamed
The shortcomings that white material viscosity that embodiment is deposited is high, poor fluidity.It is poly- in the present embodiment under the full water foamed formula of existing mainstream
Ester polyol and polyether polyol mix and match use, and foam bubble is fine and closely woven, and good stability of the dimension is also promoted to a certain extent
The anti-flammability and cementability of foam.Polyester polyol in the present embodiment is widely used at present relative to full water foamed system
Polyether polyol for, have certain cost advantage, cost performance with higher.The product is not related in raw material selection
Hazardous chemical, technique is relatively easy, securely and reliably.
The product of two above case is in foaming process without the difference on obvious time parameter.The system of the generation of foaming
One piece of rigid foam is shunk through cryogenic freezing and high-temperature baking experiment without obvious, has good dimensional stability, foam color
Milky white, abscess is fine and closely woven, uniform, hardness height (shore hardness 50~60).Indices are compared with the hardened bubble of full polyether polyol
Without significant difference.It is the general silicone oil of hard bubble that this application, which is formulated used silicone oil, it is believed that the case where using full water foamed silicone oil
Under, foaming properties will be promoted further.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of for full water foamed polyester polyol characterized by comprising binary acid or acid anhydrides, fatty acid, polyalcohol
And catalyst.
2. as described in claim 1 be used for full water foamed polyester polyol, which is characterized in that the binary acid be 120~
140 parts, the fatty acid is 40~120 parts, and the polyalcohol is 330~620 parts, and the catalyst is 0.5~2 part.
3. being used for full water foamed polyester polyol as claimed in claim 2, which is characterized in that the binary acid includes adjacent benzene
Dicarboxylic acid anhydride, the polyalcohol include the mixing of one or more of diethylene glycol, polyethylene glycol, glycerine or sorbierite
Object.
4. being used for full water foamed polyester polyol as claimed in claim 3, which is characterized in that gather described in the polyalcohol
Ethylene glycol is 200~240 parts, and the diethylene glycol is 80~140 parts, and the sorbierite is 0~160 part, and the glycerine is
50~80 parts.
5. being used for full water foamed polyester polyol as described in claim 1, which is characterized in that the fatty acid includes oil
The mixture of one or more of acid, soybean oil or palm oil.
6. being used for full water foamed polyester polyol as described in claim 1, which is characterized in that the catalyst includes metatitanic acid
The mixture of one or more of four butyl esters, stannous octoate, Dibutyltin oxide, di lauric dibutyl tin oxide.
7. a kind of for full water foamed PEPA preparation method characterized by comprising
Raw material is sent into reaction kettle, is passed through nitrogen and heat temperature raising, the raw material includes binary acid or acid anhydrides, and fatty acid is more
The pure and mild catalyst of member；
Start to stir after raw material melting, and when the temperature in the reaction kettle reaches the first preset temperature, according to institute
It states the first preset temperature and controls the reaction kettle progress heated at constant temperature；
When determining the condenser top temperature drop in the reaction kettle down to the second preset temperature, being passed through for nitrogen is closed, and right
The reaction kettle carries out vacuumize process；
When determining within the scope of the current vacuum level arrival predetermined vacuum degree in the reaction kettle, according to the current vacuum level
It controls the reaction kettle and carries out Isobarically Control, and control the reaction kettle and persistently heated with preset temperature range, until sentencing
When breaking that moisture is evaporated into the raw material, polyester polyol is taken out.
8. being used for full water foamed PEPA preparation method as described in claim 1, which is characterized in that described until sentencing
Break after the step of moisture is evaporated into the raw material, the method also includes:
Judge whether the polyester polyol in the reaction kettle meets discharging condition；
If it is not, then issuing warning note.
9. being used for full water foamed PEPA preparation method as claimed in claim 8, which is characterized in that the material strip out
It include multiple judgement parameters in part, it is described to judge whether parameter reaches for the hydroxyl value of the molecular weight of polyesters in the polyester polyol
280~300mgKOH/g, the polyester polyol acid value whether≤3mgKOH/g, the polyester polyol viscosity whether be
800~1500mPaS, the polyester polyol moisture whether less than 0.1% or the degree of functionality of the polyester polyol whether
≥3。
10. being used for full water foamed PEPA preparation method as described in claim 1, which is characterized in that described first
Preset temperature is 210 DEG C~230 DEG C, and second preset temperature is to 60~70 DEG C, and the predetermined vacuum degree range is 0.09
~0.095MPa, the preset temperature range are 220~230 DEG C.
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