CN102443130A - Biomass-based polyurethane foam containing vegetable oil residue and preparation method of biomass-based polyurethane foam - Google Patents
Biomass-based polyurethane foam containing vegetable oil residue and preparation method of biomass-based polyurethane foam Download PDFInfo
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- CN102443130A CN102443130A CN2011103246832A CN201110324683A CN102443130A CN 102443130 A CN102443130 A CN 102443130A CN 2011103246832 A CN2011103246832 A CN 2011103246832A CN 201110324683 A CN201110324683 A CN 201110324683A CN 102443130 A CN102443130 A CN 102443130A
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Abstract
The invention relates to biomass-based polyurethane foam containing vegetable oil residue, which is composed of a biomass liquification product, a catalyst, a foam stabilizer, vegetable oil residue and isocyanate. The invention also relates to a preparation method of the biomass-based polyurethane foam containing vegetable oil residue. The polyurethane foam provided by the invention has better degradation property, thus waste biomass is completely utilized and the pressure of petrochemical resources is reduced; the preparation cost is lower, and the raw materials are inexpensive, easily available and renewable; and the pore structure of the polyurethane foam material is improved and the compressive strength of the foam is improved.
Description
Technical field
The invention belongs to the chemical industry field of polymer technology, be specifically related to a kind of biomass-based polyurethane foam that contains vegetable oil residue and preparation method thereof.
Background technology
Polyurethane foam because of it has thermal characteristic and the good processing properties that specific density is little, specific tenacity is high, good, has been widely used in every field such as communications and transportation, furniture, bed accessory, building and thermal insulation as a family macromolecule material.In recent years, polyurethane foamed material has been opened up new purposes in fields such as agricultural, medical and health, the disposal of three wastes, energy-conservation, interstellar flight, national defense and military again, becomes one of kind that range of application is the widest in the material.The variation of different according to used raw material from prescription can be made into several kinds of soft, semi-rigid and rigid polyurethane foams etc.
The raw material for preparing polyurethane foamed material at present is mainly from petroleum chemicals, yet petroleum resources are exhausted day by day and oil price soars all the way, and this has all had a strong impact on the development of polyurethane industrial.And the depleted polyurethane foamed material is difficult to degraded, environment has been caused have a strong impact on.Therefore, environmental protection, biodegradable new polyurethane foam materials more and more receive people's attention, also are emphasis and the focuses of paying close attention to recently.Chinese patent CN101250329A discloses a kind of crop straw-polyurethane foam composite material; In the conventional polyurethanes foam, added crop material; The matrix material that obtains not only keeps the performance of polyurethane foam, can also effectively utilize Biological resources, is beneficial to environment protection.Chinese patent CN 102206320A discloses a kind of biomass-based polyurethane foam, and biomass wherein are the liquefied product of crop material and industrial lignin.
Summary of the invention
For overcoming of the dependence of existing polyurethane foamed material raw material to petroleum chemicals, further reduce raw materials cost, and alleviate environmental stress, the purpose of this invention is to provide a kind of biomass-based polyurethane foam that contains vegetable oil residue.
Another object of the present invention provides the said preparation method who contains the biomass-based polyurethane foam of vegetable oil residue.
The said biomass-based polyurethane foam that contains vegetable oil residue is grouped into by the one-tenth of following weight part:
50～65 parts of biomass liquefying things;
0.4～0.6 part of catalyzer;
0.5～0.65 part of suds-stabilizing agent;
5～10 parts of vegetable oil residues;
50～75 parts of isocyanic ester.
Said catalyzer is amines catalyst and metal species mixture of catalysts.
Said amines catalyst is selected from N, N-dimethylcyclohexylamine, trolamine, triethylamine, N, one or more in the N-dimethylethanolamine; Said metal species catalyzer is selected from one or more in stannous octoate, Potassium ethanoate, the dibutyl tin laurate.
Preferably, said catalyzer is made up of 0.1～0.5 part of dibutyltin dilaurate and 0.1～0.3 part of triethylamine by weight.
Said suds-stabilizing agent is selected from one or more in methyl-silicone oil, tween-80, Tween-60, the silicone oil.
Said vegetable oil residue is selected from one or more in the vegetable seed dregs of fat, the soybean dregs of fat.
Said isocyanic ester is selected from a kind of in polymethylene multi-phenenyl isocyanate, tolylene diisocyanate or the diphenylmethanediisocyanate.
The preferred polymethylene multi-phenenyl isocyanate of the present invention (PAPI) is dark-brown liquid, and functionality is 2.6～2.7, and isocyano-content is 30.5%～32.0%, and flash-point is 230 ℃, and burning-point is 245 ℃ of trade mark PM-200.
Said biomass liquefying thing is selected from corn straw, rice straw, corn cob, cotton stalk, the soybean stalk one or more liquefaction thing.
Said biomass liquefying thing can like the disclosed preparation method of Chinese patent CN102206320A, also can prepare according to following method according to prior art for preparing, and the preparation of said biomass liquefying thing may further comprise the steps:
(1) the depleted biomass is crushed to below 20 orders, is dried to constant weight;
(2) liquefaction solvent of 160～200 weight parts and 3～8 parts liquefied catalytic are mixed, be heated to 150 ℃～180 ℃;
(3) biomass after 50～80 parts of pulverizing are added wherein, stirring reaction 30～100min, reaction finishes postcooling, and the acid in the said liquefaction thing that neutralizes is removed moisture and is promptly got.
Wherein, the said liquefaction solvent of step (1) is selected from one or more in polyoxyethylene glycol, USP Kosher, NSC 11801, the terepthaloyl moietie, and preferred weight ratio is a PEG 400: USP Kosher=2～4: 1 mixed liquefied solvent; Said deliquescence accelerant is the vitriol oil of concentrated hydrochloric acid or concentration 98%.
In the said step (3), add among 4～10 parts of MgO with said liquefaction thing in acid, remove moisture at 100～150 ℃ of held 10～15h then.
The preparation method who contains the biomass-based polyurethane foam of vegetable oil residue provided by the invention may further comprise the steps:
(1) successively biomass liquefying thing, catalyzer, suds-stabilizing agent and vegetable oil residue are joined in the reactor drum, mix;
(2) again isocyanic ester is joined in the reactor drum, be stirred to oyster white and rise, pour the 20～100s that foams in the mould into;
(3) after foaming finishes,, promptly get said polyurethane foam at 20～100 ℃ of following slaking 15～30h.
Polyurethane foamed material provided by the invention, its density is at 90-130kg/m
3Between, compressive strength can reach 88-730kPa, and thermal conductivity can be used as fine lagging material and fire retardant material less than 0.04w/ (m ℃).Comparing said polyurethane foamed material with existing polyurethane foamed material has the following advantages:
(1) polyurethane foamed material according to the invention has the tangible value of environmental protection, because most of waste agronomic crop that adopts in the raw material, therefore, the polyurethane foamed material that obtains has biodegradability preferably, helps environment protection; Make full use of depleted biomass such as agricultural crop straw, corn cob etc., alleviated the pressure of petrochemical industry resource simultaneously.
(2) cost is lower, and biomass waste and vegetable oil residue are cheap and easy to get, and is renewable resources, has significantly reduced cost on the whole.
(3) improve the foam structure of polyurethane foamed material, improved the foamy compressive strength.
Embodiment
Following examples are used to explain the present invention, but are not used for limiting scope of the present invention.
Embodiment 1
The preparation of liquefaction thing:
Be that 98% vitriol oil joins in the there-necked flask with 160 parts of PEG 400s, 40 parts of USP Kosher and 5 parts of concentration by weight; Stir; Then there-necked flask is put into and be heated to 160 ℃ in the oil bath pan; Add the corn cob of 50 parts of pulverizing, stirring reaction 90min cools off with cold water after the taking-up immediately.Then in liquefied product, add 5 parts of MgO, unnecessary acid neutralizes.Then with liquefied product at 105 ℃ of held 12h, to remove moisture.
Material:
The A component comprises: 55 parts of corn cob liquefied product; 0.16 part triethylamine; 0.3 part dibutyl tin laurate; 0.58 part silicone oil;
The B component comprises 8.37 parts of vegetable seed dregs of fat;
The C component comprises 63 parts of PAPI PM-200.
The preparation method:
1) at room temperature, each raw material in the A component is added in the reactor drum mix earlier, stir;
2) again the B component is added the A component, stir fast, mix;
3) the C component is poured into rapidly in the A component, under the rotating speed of 1000-1100r/min, stirred, rise until oyster white; Be poured into immediately in the mould, natural foaming 70s at room temperature, treat that foaming finishes after; It at 60 ℃ of following slaking 4h, is at room temperature placed and made its abundant slaking in 24 hours.
The polyurethane foamed material density that makes is 121.8kg/m
3, compressive strength 730kPa, thermal conductivity 0.04W/ (m ℃).
Embodiment 2
The preparation of liquefaction thing:
With 140 parts of PEG 400s, 40 parts of USP Kosher and 5.7 parts of concentration is that 98% vitriol oil joins in the there-necked flask; Stir, there-necked flask is put into be heated to 170 ℃ in the oil bath pan then, add the straw of 60 parts of pulverizing; Stirring reaction 50min cools off with cold water after the taking-up immediately.Then in liquefied product, add 6 parts of MgO, unnecessary acid neutralizes.Then with liquefied product at 110 ℃ of held 10h, to remove moisture.
Material:
The A component comprises: 52 parts of straw liquefied product; 0.16 part triethylamine; 0.29 part dibutyl tin laurate; 0.51 part silicone oil;
The B component comprises 5.25 parts of vegetable seed dregs of fat;
The C component comprises 53 parts of PAPI PM-200.
The preparation method:
1) at room temperature, each raw material in the A component is added in the reactor drum mix earlier, stir;
2) again the B component is added the A component, stir fast, mix;
3) the C component is poured into rapidly in the A component, under the rotating speed of 1000-1100r/min, stirred, rise until oyster white; Be poured into immediately in the mould, natural foaming 20s at room temperature, treat that foaming finishes after; It at 60 ℃ of following slaking 4h, is at room temperature placed and made its abundant slaking in 24 hours.
The polyurethane foamed material density that makes is 91.56kg/m
3, compressive strength 272.19kPa, thermal conductivity 0.0394W/ (m ℃).
Embodiment 3
The preparation of liquefaction thing:
With 112 parts of PEG 400s, 48 parts of USP Kosher and 5.3 parts of concentration is that 98% vitriol oil joins in the there-necked flask; Stir, there-necked flask is put into be heated to 150 ℃ in the oil bath pan then, add the straw of 80 parts of pulverizing; Stirring reaction 60min cools off with cold water after the taking-up immediately.Then in liquefied product, add 4.6 parts of MgO, unnecessary acid neutralizes.Then with liquefied product at 130 ℃ of held 15h, to remove moisture.
Material:
The A component comprises: 65 parts of straw liquefied product; 0.21 part triethylamine; 0.34 part dibutyl tin laurate; 0.61 part silicone oil;
The B component comprises 6.1 parts of vegetable seed dregs of fat;
The C component comprises 74 parts of PAPI PM-200.
The preparation method:
1) at room temperature, each raw material in the A component is added in the reactor drum mix earlier, stir;
2) again the B component is added the A component, stir fast, mix;
3) the C component is poured into rapidly in the A component, under the rotating speed of 1000-1100r/min, stirred, rise until oyster white; Be poured into immediately in the mould, natural foaming 100s at room temperature, treat that foaming finishes after; It at 60 ℃ of following slaking 4h, is at room temperature placed and made its abundant slaking in 24 hours.
The polyurethane foamed material density that makes is 129.16kg/m
3, compressive strength 88.63kPa, thermal conductivity 0.0372W/ (m ℃).
Though, the present invention has been done detailed description in the preceding text with general explanation and specific embodiments, on the basis of the present invention, can to some modifications of do or improvement, this is conspicuous as far as these those skilled in the art.Therefore, these modifications or the improvement on the basis of not departing from spirit of the present invention, made all belong to the scope that requirement of the present invention is protected.
Claims (10)
1. a biomass-based polyurethane foam that contains vegetable oil residue is characterized in that, is grouped into by the one-tenth of following weight part:
50～65 parts of biomass liquefying things;
0.4～0.6 part of catalyzer;
0.5～0.65 part of suds-stabilizing agent;
5～10 parts of vegetable oil residues;
50～75 parts of isocyanic ester.
2. polyurethane foam according to claim 1; It is characterized in that said catalyzer is amines catalyst and metal species mixture of catalysts, said amines catalyst is selected from N; N-dimethylcyclohexylamine, trolamine, triethylamine, N, one or more in the N-dimethylethanolamine; Said metal species catalyzer is selected from one or more in stannous octoate, Potassium ethanoate, the dibutyl tin laurate; Said catalyzer is preferred by weight by 0.1～0.5 part of dibutyltin dilaurate and 0.1～0.3 part of mixture that triethylamine is formed.
3. polyurethane foam according to claim 1 is characterized in that said suds-stabilizing agent is selected from one or more in methyl-silicone oil, tween-80, Tween-60, the silicone oil.
4. polyurethane foam according to claim 1 is characterized in that, said vegetable oil residue is selected from one or more in the vegetable seed dregs of fat, the soybean dregs of fat.
5. polyurethane foam according to claim 1 is characterized in that, said isocyanic ester is selected from a kind of in polymethylene multi-phenenyl isocyanate, tolylene diisocyanate or the diphenylmethanediisocyanate.
6. polyurethane foam according to claim 1 is characterized in that, said biomass liquefying thing is selected from corn straw, rice straw, corn cob, cotton stalk, the soybean stalk one or more liquefaction thing.
7. polyurethane foam according to claim 6 is characterized in that, the preparation of said biomass liquefying thing may further comprise the steps:
(1) the depleted biomass is crushed to below 20 orders, is dried to constant weight;
(2) liquefaction solvent of 160～200 weight parts and 3～8 parts liquefied catalytic are mixed, be heated to 150 ℃～180 ℃;
(3) biomass after 50～80 parts of pulverizing are added wherein, stirring reaction 30～100min, reaction finishes postcooling, and the acid in the said liquefaction thing that neutralizes is removed moisture and is promptly got.
8. polyurethane foam according to claim 7; It is characterized in that; The said liquefaction solvent of step (1) is selected from one or more in polyoxyethylene glycol, USP Kosher, NSC 11801, the terepthaloyl moietie, and preferred weight ratio is a PEG 400: USP Kosher=2～4: 1 mixed liquefied solvent; Said deliquescence accelerant is the vitriol oil of concentrated hydrochloric acid or concentration 98%.
9. polyurethane foam according to claim 7 is characterized in that, in the said step (3), add among 4～10 parts of MgO with said liquefaction thing in acid, remove moisture at 100～150 ℃ of held 10～15h then.
10. the preparation method of each said polyurethane foam of claim 1-9 is characterized in that, may further comprise the steps:
(1) successively biomass liquefying thing, catalyzer, suds-stabilizing agent and vegetable oil residue are joined in the reactor drum, mix;
(2) again isocyanic ester is joined in the reactor drum, be stirred to oyster white and rise, pour the 20～100s that foams in the mould into;
(3) after foaming finishes,, promptly get said polyurethane foam at 20～100 ℃ of following slaking 15～30h.
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Cited By (8)
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| CN103626948A (en) * | 2013-11-26 | 2014-03-12 | 北京联合大学生物化学工程学院 | Polyurethane foam material synthesized from plant polyols |
| CN104877359A (en) * | 2015-05-05 | 2015-09-02 | 汪青 | Corn asphalt, corn resin and zeaxanthin binder prepared from kettle residue |
| CN106675070A (en) * | 2016-12-30 | 2017-05-17 | 深圳市泽青源科技开发服务有限公司 | Fungus-based biomass fireproof material with wheat straw as main material and preparation method thereof |
| CN106675069A (en) * | 2016-12-30 | 2017-05-17 | 深圳市泽青源科技开发服务有限公司 | Fungus-based biomass fireproof material taking rice straw as main ingredient and preparation method thereof |
| CN108264916A (en) * | 2017-12-25 | 2018-07-10 | 北京三聚环保新材料股份有限公司 | A kind of one kettle way liquefaction process of biomass |
| CN111019331A (en) * | 2019-12-24 | 2020-04-17 | 齐鲁工业大学 | Polyester elastomer film and preparation method thereof |
| US10975312B2 (en) | 2017-12-25 | 2021-04-13 | Beijing Sanju Environmental Protection & New Materials Co., Ltd | Process for one-pot liquefaction of biomass or coal and biomass |
| CN114805732A (en) * | 2022-06-11 | 2022-07-29 | 朱睿萍 | Preparation method of biodegradable polyurethane foam material |
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| US10975312B2 (en) | 2017-12-25 | 2021-04-13 | Beijing Sanju Environmental Protection & New Materials Co., Ltd | Process for one-pot liquefaction of biomass or coal and biomass |
| CN111019331A (en) * | 2019-12-24 | 2020-04-17 | 齐鲁工业大学 | Polyester elastomer film and preparation method thereof |
| CN111019331B (en) * | 2019-12-24 | 2021-11-02 | 齐鲁工业大学 | Polyester elastomer film and preparation method thereof |
| CN114805732A (en) * | 2022-06-11 | 2022-07-29 | 朱睿萍 | Preparation method of biodegradable polyurethane foam material |
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Application publication date: 20120509 |