CN101240055A - Method for preparing low VOC content polyurethane foam and use thereof - Google Patents
Method for preparing low VOC content polyurethane foam and use thereof Download PDFInfo
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- CN101240055A CN101240055A CNA2008101018721A CN200810101872A CN101240055A CN 101240055 A CN101240055 A CN 101240055A CN A2008101018721 A CNA2008101018721 A CN A2008101018721A CN 200810101872 A CN200810101872 A CN 200810101872A CN 101240055 A CN101240055 A CN 101240055A
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- polyurethane foam
- isocyanic ester
- content
- polyether glycol
- low volatile
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- 229920005830 Polyurethane Foam Polymers 0.000 title claims abstract description 73
- 239000011496 polyurethane foam Substances 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims description 19
- 239000012855 volatile organic compound Substances 0.000 claims abstract description 96
- 229920000570 polyether Polymers 0.000 claims abstract description 81
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 77
- 229920000642 polymer Polymers 0.000 claims abstract description 41
- 229920002545 silicone oil Polymers 0.000 claims abstract description 41
- 239000012948 isocyanate Substances 0.000 claims abstract description 34
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 34
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 239000006260 foam Substances 0.000 claims abstract description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 150
- 150000002148 esters Chemical class 0.000 claims description 75
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 75
- 239000003795 chemical substances by application Substances 0.000 claims description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 41
- -1 alcohol compound Chemical class 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 10
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 10
- 229960004418 trolamine Drugs 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000007634 remodeling Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 230000000704 physical effect Effects 0.000 abstract description 18
- 229920005862 polyol Polymers 0.000 abstract description 5
- 150000003077 polyols Chemical class 0.000 abstract description 5
- 230000002633 protecting effect Effects 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000003431 cross linking reagent Substances 0.000 abstract 1
- 238000005034 decoration Methods 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 23
- 239000000463 material Substances 0.000 description 23
- 239000000126 substance Substances 0.000 description 19
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 18
- 150000001875 compounds Chemical group 0.000 description 15
- 238000012360 testing method Methods 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 229920002635 polyurethane Polymers 0.000 description 8
- 239000004814 polyurethane Substances 0.000 description 8
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- 239000003208 petroleum Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 4
- 206010019233 Headaches Diseases 0.000 description 4
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 231100000739 chronic poisoning Toxicity 0.000 description 4
- 238000005187 foaming Methods 0.000 description 4
- 230000014509 gene expression Effects 0.000 description 4
- 231100000869 headache Toxicity 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 150000002483 hydrogen compounds Chemical class 0.000 description 4
- 238000006552 photochemical reaction Methods 0.000 description 4
- 229920001228 polyisocyanate Polymers 0.000 description 4
- 239000005056 polyisocyanate Substances 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000002607 hemopoietic effect Effects 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- 206010010071 Coma Diseases 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 229920000265 Polyparaphenylene Polymers 0.000 description 2
- 231100000570 acute poisoning Toxicity 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 208000010668 atopic eczema Diseases 0.000 description 2
- 230000002567 autonomic effect Effects 0.000 description 2
- 210000003169 central nervous system Anatomy 0.000 description 2
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 2
- 208000002173 dizziness Diseases 0.000 description 2
- 230000004064 dysfunction Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 2
- 229910052919 magnesium silicate Inorganic materials 0.000 description 2
- 235000019792 magnesium silicate Nutrition 0.000 description 2
- 239000000391 magnesium silicate Substances 0.000 description 2
- 208000007106 menorrhagia Diseases 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 208000024891 symptom Diseases 0.000 description 2
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 2
- 239000003039 volatile agent Substances 0.000 description 2
- 230000008673 vomiting Effects 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- KZEVSDGEBAJOTK-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[5-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CC=1OC(=NN=1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O KZEVSDGEBAJOTK-UHFFFAOYSA-N 0.000 description 1
- GTEXIOINCJRBIO-UHFFFAOYSA-N 2-[2-(dimethylamino)ethoxy]-n,n-dimethylethanamine Chemical class CN(C)CCOCCN(C)C GTEXIOINCJRBIO-UHFFFAOYSA-N 0.000 description 1
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 1
- 208000032467 Aplastic anaemia Diseases 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 206010009192 Circulatory collapse Diseases 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 206010012434 Dermatitis allergic Diseases 0.000 description 1
- 206010020565 Hyperaemia Diseases 0.000 description 1
- 206010067125 Liver injury Diseases 0.000 description 1
- UEEJHVSXFDXPFK-UHFFFAOYSA-O N-dimethylethanolamine Chemical compound C[NH+](C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-O 0.000 description 1
- 208000002193 Pain Diseases 0.000 description 1
- 206010039203 Road traffic accident Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- 206010041349 Somnolence Diseases 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
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- 238000004458 analytical method Methods 0.000 description 1
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- 235000019789 appetite Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 201000008937 atopic dermatitis Diseases 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- IFVTZJHWGZSXFD-UHFFFAOYSA-N biphenylene Chemical group C1=CC=C2C3=CC=CC=C3C2=C1 IFVTZJHWGZSXFD-UHFFFAOYSA-N 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
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- 230000036541 health Effects 0.000 description 1
- 231100000753 hepatic injury Toxicity 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
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Landscapes
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to polyurethane foam with low content of volatile organic compound, preparation and application thereof. The preparation includes: using retreated polyether polyol, polymer polyol with low content of volatile matter, foamer, catalyst with little smell, crosslinking agent, low fogging silicone oil and isocyanate with low content of volatile matter as raw material, mixing according to a definite proportion, introducing the mixture into iron mould at the temperature of 45-50 DEG C., demoulding, forming the foam product at the temperature of 20-30 DEG C. after demoulding, detecting. The invention carries out treatment of polyether polyol, de novo synthesis of polymer polyol and optimized selection of isocyanate to prepare polyurethane foam with low content of volatile organic compound. Advantages of the invention are greatly reduction of VOC content, enhancing environmental protecting effect, improved physical property of produced polyurethane foam. The inventive polyurethane foam is mainly used in decoration in automobile, and also can be used for indoor sofa, bedclothing, lining and so on.
Description
Technical field
The present invention relates to the foaming method and the purposes of macromolecular material, specifically the Preparation method and use of the polyurethane foam of low organic volatile VOC (volatile organic compounds) content relates to the synthetic of low VOC raw material simultaneously.
Prior art
Prior art in the presence of whipping agent, catalyzer, siloxanes tensio-active agent (being commonly called as silicone oil) and other auxiliary agents, by organic isocyanate with contain compound bearing active hydrogen reaction and produce polyurethane foam.Contain compound bearing active hydrogen and comprise polyether glycol, polymer polyatomic alcohol, polyamine, He Shui.In the preparation polyurethane foam, catalyzer has promoted two main reactions, i.e. gel and foaming.These are reflected in the technological process and carry out simultaneously, and are in the competitive equilibrium relation, produce to have the polyurethane foam of desired physical properties.
Because the physicals that they are outstanding, polyurethane foam is used for extensive fields.The market of particularly important is automotive industry.Polyurethane foam is usually used in the automobile as roof liner, and the inside of door covers, and as tinted shade, dashboard, bearing circle, and is used for seating systems.
The automaker is obviously strict more to the demand that its foam supplier proposes in recent years, and particularly the foamy emission standard is carried out assay determination to organic volatile (VOC) content now.
Show that according to some compellent data the healthy of person for driving a car in the in-vehicle exposure serious threat.China room air monitoring center of upholstery association 2006 is detected 200 cars, found that, if with reference to the IAQ (indoor air quality) standard, there is nearly 90% automobile all to have in the car formaldehyde or benzene content overproof problem in the air, and most of vehicle formaldehyde exceeds standard all more than five or six times, and wherein the Air quality in the new car is the poorest.
Show Detection of Air Quality result in the homemade new car car of formal announcement in the end of the year 2006 of Country Geological Experimental Testing Center according to disclosed material, in 20 brands accepting to detect, 3 months homemade new car of 50 sections of listings, only there is the detection of 5 harmful elements in the 9 sedans cars qualified fully.Country Geological Experimental Testing Center is one of the national industry analysis of 13 under Ministry of Science and Technology test center, this time harmful element is respectively formaldehyde, benzene-like compounds and other VOC in 5 cars that detect, wherein the phenomenon that exceeds standard of formaldehyde is the most serious, and the air formaldehyde content surpasses the indoor formaldehyde world value of limiting the quantity of in 82% the tested new car car; The benzene in air kind compound content exceeds standard in 28% the tested new car car.
Meaning released in VOC Chinese: organic volatile, have the flavor of smelling, and pungency is arranged, and most compound has genotoxicity.Think that at present VOC can cause the immunity of organism off-leveling, influences central nervous system function, dizziness, headache, subjective symptoms such as drowsiness, unable, uncomfortable in chest occur; Also may influence Digestive tract, poor appetite occur, feel sick etc., but transformation reactions etc. appears in liver injury and hemopoietic system when serious.
Principal pollutant and harm in the car:
Formaldehyde: be irritant gas colourless, that have overpowering odor, the aqueous solution common name formalin of its 35%-40%, the a small amount of formaldehyde of normal suction can cause chronic poisoning, mucous hyperemia, skin irritation disease, allergic dermatitis, nail angling and fragility, nail matrix finger tip pain etc. occur.Constitutional symptom have headache, weak, that stomach is received is poor, palpitaition, have a sleepless night, lose weight and autonomic nervous dysfunction etc.
Benzene-like compounds comprises: benzene,toluene,xylene etc. are a kind of colourless, pleasantly sweet transparent liquid at normal temperatures, and have the intensive aromatic odour.High density benzene has anesthetic action to central nervous system, causes acute poisoning; Long-term contact benzene has infringement to hemopoietic system, causes chronic poisoning.Acute poisoning: the lighter has headache, dizziness, feels sick, vomiting, slight excited, intoxication such as lurch; Severe patient is gone into a coma, tic, blood pressure drops, so that breathes and circulatory failure.Chronic poisoning: main performance has neurasthenic syndrome; Hemopoietic system changes: white corpuscle, thrombopenia, and aplastic anemia appears in weight person; Leukemia (with acute myelogenous for seeing) can take place in the minority case more after chronic poisoning; Skin lesion has degreasing, drying, chaps, dermatitis; Can cause hyper-menorrhea with menostaxis.
Other pollutents: as amine, low mass molecule alcohol class; The volatility benzene-like compounds that contains trace in the isocyanic ester has headache, weak, state such as vomit, lurch, and severe patient is gone into a coma.Also can cause allergic, autonomic nervous dysfunction etc.
Above pollutent is not all from polyurethane foamed material, but the organic volatile that undeniable polyurethane foamed material discharges also is one of source of pollution.
In the polyurethane foamed material there be main raw material: polyether glycol, polymer polyatomic alcohol, catalyzer, silicone oil, whipping agent, linking agent and isocyanic ester, the volatile matter that contains following trace: formaldehyde, benzene-like compounds and other organic volatiles at first have micro-aldehyde compound in the manufacturing processed own in the polyether glycol; The volatility benzene-like compounds such as vinylbenzene that secondly trace is arranged in the raw material that polymer polyatomic alcohol uses; Other organic volatiles that contain trace in catalyzer, silicone oil and the catalyzer are as amine, low mass molecule alcohol class; Therefore the volatility benzene-like compounds that contains trace in the isocyanic ester will reduce VOC content in the polyurethane material, needs to select or transform the polyurethane foam starting material, could reduce the existence of organic volatile effectively.
Along with popularizing of automobile family oriented, the Air quality quality is paid attention to by people gradually in the car, car Air quality quality not only influences the healthy of person for driving a car, and traffic exerted an influence, even traffic accident appears, influence person for driving a car and pedestrian's life, the upholstery of environmental protection is extremely urgent, has come into each car owners's life.
Since in the GB to the unified standard of organic volatile content none of polyurethane material, the inventor carries out with reference to the internal standard of some automobile production producers and the standard of standard GB 18586-2001 " limits of harmful substances in the house decorative material polyvinyl chloride sheet floor ", the standard that this standard is carried out be organic volatile (VOC) content less than 35ppm, some auto vendors fix on organic volatile (VOC) content less than 25ppm with standard.Country is revising the examination criteria of the VOC of indoor (containing automobile-used) polyurethane material again, and the polyurethane foam of therefore producing low VOC is very urgent.The present invention with standard GB 18586-2001 " limits of harmful substances in the house decorative material polyvinyl chloride sheet floor " as examination criteria and detection method.
VOC is the english abbreviation of organic volatile (volatile organic compounds).Its definition has several, and for example, U.S. ASTM D3960-98 standard is defined as any organic compound that can participate in atmospheric photochemical reaction with VOC.The definition of the United States Federal's Environmental Protection Administration (EPA): organic volatile is except that CO, CO2, H2CO3, metallic carbide, metal carbonate and volatile salt, the carbon compound of any participation atmospheric photochemical reaction.(the WHO of the World Health Organization, 1989) total organic volatile (TVOC) is defined as, fusing point is lower than room temperature and the general name of the organic volatile of boiling point between 50～260 ℃, and the most general common recognition thinks that VOC is meant that those boiling points are equal to or less than 250 ℃ chemical substance.The definition of these VOC is divided into two classes, and a class is the VOC definition on the common meaning, only illustrates what is organic property volatile matter, or is volatile organic matter under what conditions; Another kind of is definition on the environment protection significance, that is to say, and be active that class volatile organic matter, promptly can produce that class volatile organic matter of harm.Very obvious, from environment protection significance, volatilization and these 2 of atmospheric photochemical reactions of participation are crucial.Non-volatile or do not participate in atmospheric photochemical reaction and just not constitute harm.The present invention is according to present status in China, stipulate according to standard GB 18586-2001, select comparatively strict VOC definition, fusing point is lower than room temperature and the general name of the organic volatile of boiling point between 50～260 ℃, comprise benzene,toluene,xylene and other volatile organic contents, its VOC total amount of this standard code is less than 35ppm.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, obvious reduction foamy organic volatile content is provided, the method and the purposes of the high resilience moulded foam of excellent stability and the polyurethane foam of outstanding physicals particularly are fit to automotive trim and indoor polyurethane material.
The object of the invention realizes by following measure:
The preparation method of the polyurethane foam of low volatile organic compound content, raw material is the polyether glycol of handling again, polymer polyatomic alcohol, whipping agent, low smell catalyzer, linking agent, low atomizing silicone oil and the low volatile content isocyanic ester of low volatile content;
The polyvalent alcohol compound comprises polyether glycol, polymer polyatomic alcohol, whipping agent, catalyzer, linking agent and silicone oil;
Polyvalent alcohol compound raw material weight ratio is:
Polyether glycol: 38.1-57.2
Polymer polyatomic alcohol: 37.9-56.1
Whipping agent: 2.5-2.7
Catalyzer: 1.1-1.3
Linking agent: 0.8-1.1
Silicone oil: 0.5-0.7
Ratio is between each raw material: isocyanic ester and polyvalent alcohol compound equivalence ratio are 0.90-1.40, and promptly isocyanate index is 90-140;
The preparation method of polyurethane foam is:
1) in stainless steel vessel A, with polyether glycol, polymer polyatomic alcohol, catalyzer, silicone oil, whipping agent and linking agent, press raw material weight than adding successively, stir, make the polyvalent alcohol compound, placed 3 minutes;
2) in stainless steel vessel B, calculate and weighing isocyanic ester weight according to isocyanate index, to mix, temperature is controlled at 22-23 ℃;
3) take out a certain amount of 1 then) the polyvalent alcohol compound, with 2) isocyanate component pours in the polyvalent alcohol compound, and stirs short mix 6-8 second rapidly;
4) with 3) pour in the swage tool, temperature is controlled at 45 ℃-50 ℃, the demoulding in 4-6 minute;
5) foam sample after the depanning under 20-30 ℃, is placed aging moulding after 24 hours, detects.
Reduce foamy VOC discharge content for reaching, the GB18586-2001 law regulation that is up to state standards must be to the raw-material transformation of urethane.
Purpose of the present invention provides the method that polyether glycol is handled again, reduces the content of VOC in the polyether glycol.
Again the method for handling polyether glycol is as follows:
In reactor, by weight percentage, add polyether glycol 330N 96%-98%, add finishing agent 0.1-0.3%, deionized water 1.9%-3.9%, be warming up to 80 ℃-90 ℃ again, stirred reduced vacuum 30 minutes, temperature is controlled at 105 ℃-110 ℃, moisture is less than 0.02-0.04%, and the circulating filtration discharging promptly obtains the polyether glycol product that the technology of the present invention is handled.
Another object of the present invention provides the low VOC content polymer polyatomic alcohol, makes VOC discharge content significantly reduce, and keeps the physicals of polyurethane foam excellence simultaneously.
The polymer polyatomic alcohol method of low volatile content is as follows:
In reactor, by weight percentage, add polyether glycol 330N-1 75-85%, trolamine 5-8%, temperature is at 20-50 ℃, and 40-70 adds thick MDI 8.5-14% fast in second, add diethanolamine 1.5-3% subsequently, mixed 1-2 hour, temperature is reduced to 30-40 ℃ with bottom discharge, promptly gets synthetic low volatile content polymer polyatomic alcohol product of the present invention.
Whipping agent is: deionized water, methylene dichloride, pentane, fluorine Lyons; Preferred deionized water.
Select or mix low volatile content aminated compounds catalyzer to be: A-1, A-33, C-225, a kind of or two or more mixtures wherein; Preferred catalyst is: A-1, A-33, the two or more mixtures of C-225.
Linking agent is: diethanolamine and trolamine.
Select low atomizing silicone oil to be: L-3015, L-3415, the Y-10366 of U.S. Niax company; Execute B8734LF with German Gao Shi Mitt USA Corporation with German height; Preferred B8734LF.
Another object of the present invention provides a kind of mixed type isocyanate material, and this mixed type isocyanate material not only makes the VOC discharge significantly reduce, and keeps the physicals of polyurethane foam excellence simultaneously.
Isocyanic ester comprises aliphatics, alicyclic, araliphatic, aromatic polyisocyanate.Isocyanic ester has: 2.4 and 2.6-tolylene diisocyanate 80/20, be TDI80/20, the diphenylene vulcabond, be smart MDI, the polyphenylene polyisocyanates, be thick MDI, remodeling isocyanic ester manufacturing enterprise: the 103C of BASF Aktiengesellschaft, Yantai ten thousand China 1630, the remodeling isocyanic ester 2424 that steps of U.S.'s Hensel etc., the mixed type isocyanic ester mainly contains the BX118 etc. of TM20, TM30, TM50 and Korea S's brocade lake Mitsui of Japanese NPU company.
The isocyanic ester that the present invention selects for use has: TDI80/20, thick MDI, mixed type isocyanic ester be Japanese NP company's T M20 and remodeling isocyanic ester be Hensel step 2424, the BX118 of Korea S's brocade lake Mitsui.
The preparation method of isocyanic ester compound of the present invention is: according to weight percent, with 20-30%TM20, the mixture of thick MDI of 5-15% and 65-75%BX118 stirred 1 hour, was the isocyanic ester compound.The present invention proportionally, with TM20, the isocyanic ester compound that thick MDI and remodeling isocyanic ester BX-118 make gets an unexpected result, the VOC content of polyurethane foam is low.
The purposes of the polyurethane foam of low volatile organic compound content mainly is used in the motor vehicle interior trim, also can be used for indoor sofa, bedding, liner etc.
The present invention produces the necessary starting material of polyurethane foamed material polyether glycol, polymer polyatomic alcohol, whipping agent, catalyzer, silicone oil, linking agent and isocyanic ester.For the minimizing of the VOC content that guarantees polyurethane foam and do not influence the original good performance of its foam, the present invention sets about transforming from each raw material, transformation has three kinds of approach, one, change material of the same type, as: the specific combination of selecting the catalyzer of low VOC content, low atomizing silicone oil and isocyanate mixture; Two, the processing again of raw material reduces the VOC content of this raw material, as: the processing again of polyether glycol, stably reduce the existence of volatile organic compounds; Three, synthetic again similar product is as synthesizing of low VOC content polymer polyatomic alcohol.Polymkeric substance in the common polymer polyatomic alcohol is the polymkeric substance or the autopolymer of vinylbenzene, vinyl cyanide, contain the existence of a certain amount of free vinylbenzene, vinyl cyanide or volatile small molecules vinylbenzene and vinyl cyanide self-aggregate residue, and the present invention adopts many phenyl-polymethylenes-polyisocyanates (thick MDI) of low VOC and trolamine, diethanolamine polymkeric substance, greatly reduces the existence of organic volatile in the polymkeric substance.
Through transformation of the present invention, unexpectedly to produce and have still less high resilience (HR) polyurethane foam of VOC content, its VOC total amount is below 35ppm, and is even lower.Catalyzer, low atomizing silicone oil material and the mixed type isocyanic ester provided by the invention of the low organic volatile content that polyether glycol, the polymer polyatomic alcohol that uses the technology of the present invention production, the use the present invention who uses the present invention to handle selects or the polyurethane foam of the isocyanic ester manufacturing of retrofiting.For guaranteeing the complete slaking of this foam materials, all place censorship survey unit after 24 hours.
The definition of isocyanate index (Iso index): isocyanate index is an empirical value, is a polyurethane foam reaction parameter commonly used, also is a basic parameter of polyurethane foam prescription.According to the equivalent principle, active hydrogen compounds complete reaction in isocyanic ester and the polyvalent alcohol compound, equivalence ratio should be 1.00, and this equivalent ratio is referred to as isocyanate index, and promptly isocyanate index was 100 (also can represent with 1.00).The unification of the application's isocyanate index is 100 expressions.
Through calculating, isocyanate index is 102, and the polyvalent alcohol compound is 100g, and the add-on of isocyanic ester B is 39.2g.
But consider foamy flexibility, intensity and structure etc., actual general isocyanate index is can be between 90～140.If isocyanate index is 105, then represent isocyanic ester excessive 5%.
The concrete calculating means of isocyanate index: according to the equivalent reaction principle, isocyanic ester and the compound complete reaction that contains reactive hydrogen, be isocyanic ester and all contain hydroxyl or amino compound equivalent reaction in same reaction, principle calculates the isocyanic ester consumption in view of the above.The quality of the active dydrogen compounds isocyanic ester that component consumes of every element quality is calculated in general employing respectively, and the method for summation again calculates the total flow of isocyanic ester, i.e. total consumption of isocyanic ester.When urethane foam formulating of recipe or expression, be benchmark with 100 gram mass polyvalent alcohol compounds usually, calculate the gram mass of the isocyanic ester of consumption, i.e. the consumption of isocyanic ester.
Amount (g) basic calculating formula of every kind of isocyanic ester that compound consumes that contains reactive hydrogen is as follows:
The consumption of isocyanic ester (g)=(÷ (the NCO%/M) * Iso/ β of N * Q)/56100
The quality g of active hydrogen compounds during N represents to fill a prescription in the formula
Q represents the hydroxyl value mgKOH/g of this active hydrogen compounds
The molar mass mg of 56100 expression KOH
NCO% represents NCO content %
M represents isocyanic ester molar mass g
β represents the purity % of isocyanic ester
Iso represents isocyanate index
The purity of isocyanic ester, the NCO content in the isocyanic ester and the molar mass of NCO are provided by supplier, generally can consult the isocyanate products quality certificate that supplier provides.
In this patent foaming formulation, active hydrogen compounds has: polyether glycol, polymer polyatomic alcohol, various catalyzer, water, silicone oil and linking agent (trolamine, diethanolamine), add this six kinds of raw materials by weight, and promptly be polyol blends.
Other purposes of the present invention select to add the low Silicon surfactant (hereinafter to be referred as silicone oil) that atomizes, and have the high resilience polyurethane foam that reduces the VOC discharge; Select to add the catalyzer of low VOC content, have the high resilience polyurethane foam that reduces the VOC discharge.
Final purpose of the present invention provides the method with the polyurethane foam that reduces the VOC discharge, be specially adapted to use the high resilience polyurethane foam of disposable foaming and the production of premix combination material method, and be applied to the motor vehicle interior trim, also can be used for indoor sofa, bedding, liner etc., improve the environment protecting of polyurethane foam, reach the domestic and international VOC emission standard of polyurethane foam, in addition lower.
Handling the finishing agent of polyether glycol, is atlapulgite, diatomite, Magnesium Silicate q-agent; Preferred Magnesium Silicate q-agent.
The present invention has following advantage compared to existing technology:
Result according to the VOC content of standard GB 18586-2001 method test, detect data from embodiment 1 to embodiment 9, show that the present invention synthesizes high resilience polyurethane foam and compares with common high resilience polyurethane foam, VOC content is from more than 150, reduce to below 30, reduce VOC content significantly, strengthened environment protecting.
Emphasis of the present invention is the optimized choice by the synthetic and isocyanic ester that polyether glycol has been carried out processing, novel polymer polyvalent alcohol, aid in the selection of catalyzer, silicone oil and whipping agent, reach the purpose of preparation low VOC content polyurethane foam, polyurethane foam products of the present invention mainly is used in the motor vehicle interior trim, also can be used for indoor sofa, bedding, liner etc., reduce the VOC quantity discharged of polyurethane foam, strengthen environment protecting.It is generally acknowledged that the high physicals of (except the special purpose) polyurethane foam test data is better, relatively use isocyanic ester compound of the present invention and remodeling isocyanic ester 2424 from the following examples, the physicals of isocyanic ester compound polyurethane foam is better as can be seen.
7-1 and 7-2 physicals test in the comparing embodiment, as can be seen: the physicals test data of the prepared polyurethane foam of isocyanic ester compound of the present invention, the physicals test data of the MDI that obviously is better than retrofiting.
Embodiment
The raw material that the present invention uses:
Polyether glycol 330N selects large-lot producer of domestic a few family product for use, comprising:
Tianjin petrochemical corporation (complex) the 3rd petroleum chemical plant, east, Shandong polyethers factory of big chemical industry group company, urethane division department of Shanghai Gaoqiao petrochemical corporation (complex) and Shandong Zibo moral are believed federal chemical Industrial Co., Ltd.
The polymer polyatomic alcohol that the present invention uses is selected for use: polymer polyatomic alcohol 36/28 and the present invention of Tianjin petrochemical corporation (complex) the 3rd petroleum chemical plant prepare new polymer polyatomic alcohol 36/20.
Selecting for use of whipping agent:
Deionized water
Catalyzer is selected for use:
The dipropylene glycol solution GE new high-tech material group of two (dimethylamino ethyl) ethers of A-1:70%
The dipropylene glycol solution GE new high-tech material group of A-33:33% triethylene diamine
N, N-dimethylethanolamine BASF Aktiengesellschaft
C-225 GE new high-tech material group
Linking agent is selected for use:
Diethanolamine, trolamine Dow Chemical company
Silicone oil is selected for use:
L-3015 and L-3002 GE Mitugao New Material Group
Y-10366 GE Mitugao New Material Group
B8736LF Germany Gao Shi Mitt USA Corporation
Isocyanic ester is selected for use:
Mitsui company: 2.4 and 2.6-tolylene diisocyanate (80/20) (be called for short TDI80/20);
BASF Aktiengesellschaft: polyphenylene polyisocyanates (being called for short thick MDI) M20S;
Japan NPU company: mixed type isocyanic ester TM20;
U.S. Huntsman Corporation: remodeling isocyanic ester 2424;
Korea S brocade lake Mitsui: mixed type isocyanic ester BX118.
Enumerate 7 embodiment below, to the relation between the VOC content between urethane raw of the present invention and the polyurethane foam, be illustrated, but the present invention is not limited in these embodiment.
Feedstock production
One) basic recipe and the method handled again of polyether glycol 330N '
In 5L circulation spray reactor, by weight percentage, add polyether glycol 330N 2940g, 98%, add finishing agent 4.0g, 0.13%, deionized water 56g, 1.87%, be warming up to 85 ℃～90 ℃ again, stirred 30 minutes, reduced vacuum, temperature are controlled at 105 ℃～110 ℃, moisture is less than 0.02-0.04%, the circulating filtration discharging promptly gets the product that the technology of the present invention is handled, polyether glycol 330NA.The circulating filtration discharging promptly gets the product that the technology of the present invention is handled, polyether glycol 330NA.
This manufacturer who tests used polyether glycol 330N is Tianjin petrochemical corporation (complex) the 3rd petroleum chemical plant
Two) polymer polyatomic alcohol of low volatile content of the present invention is synthetic, and operation steps is as follows;
In reactor, by weight percentage, adding MDI of the present invention is 11g, 11%, adding trolamine subsequently is 6g, 6%, mixed 1-2 hour, temperature is reduced to 30-40 ℃ of polyether glycol 330NA80g, and 80%, diethanolamine is 3g, 3%, temperature is at 35-45 ℃, and 40-70 adds slightly with bottom discharge in second fast, promptly gets low volatile content polymer polyatomic alcohol 36/20 of the present invention.Detect index: viscosity is 1600-2800mPa.s/25 ℃, moisture 0.05%-0.10%.
Three) preparation of isocyanic ester compound
Isocyanic ester D of the present invention preparation, according to weight percent, with 20g TM20,20%: 10g MDI, 10% and 70g BX118,70%, make compound, stir discharging in 1 hour, be isocyanic ester D.Detect index: NCO content is 36-40.
Below be each component numbering in embodiments of the present invention:
Following 330N polyether glycol is according to above-mentioned one) method handled again of polyether glycol 330N handles, and it is just the same to handle material therefor, usage ratio and production method, and the present invention numbers according to 330N polyether glycol manufacturer's difference:
With Tianjin petrochemical corporation (complex) the 3rd petroleum chemical plant 330N polyether glycol, according to above-mentioned one) method handled again of polyether glycol 330N handles the polyether glycol that obtains: be numbered polyether glycol 330NA-1;
With the big 330N of polyethers factory of the chemical industry group company polyether glycol in Shandong east, according to above-mentioned one) method handled again of polyether glycol 330N handles the polyether glycol that obtains: be numbered polyether glycol 330NA-2;
With the 330N of urethane division department of Shanghai Gaoqiao petrochemical corporation (complex) polyether glycol, according to above-mentioned one) method handled again of polyether glycol 330N handles the polyether glycol that obtains: be numbered polyether glycol 330NA-3;
Believe the federal chemical 330N of Industrial Co., Ltd polyether glycol with the Shandong Zibo moral, according to above-mentioned one) method handled again of polyether glycol 330N handles the polyether glycol that obtains: be numbered polyether glycol 330NA-4;
The polyether glycol 330N that adopts each big polyethers manufacturer to provide, numbering in an embodiment:
Tianjin petrochemical corporation (complex) the 3rd petroleum chemical plant: polyether glycol 330N-1;
East, Shandong polyethers factory of big chemical industry group company: polyether glycol 330N-2;
Urethane division department of Shanghai Gaoqiao petrochemical corporation (complex): polyether glycol 330N-3;
The Shandong Zibo moral is believed federal chemical Industrial Co., Ltd: polyether glycol 330N-4;
Silicone oil numbering in an embodiment:
The mixture of silicone oil a:L-3015 and L-3002 (1: 1, weight %);
The mixture of silicone oil b:Y-10366 and L-3002 (1: 1, weight %);
Silicone oil c:B8734LF;
Catalyzer numbering in an embodiment:
Catalyst A: A-1, D-33, C-225 mixture, A-1: D-33: C-225=1: 5: 4, weight %;
Catalyst B: A-1, D-33 mixture, A-1: D-33=1: 5, weight %;
Catalyzer C:A-1, D-33 and N, N-dimethyl ethanol amine mixt, A-1: D-33: N, N-dimethylethanolamine=1: 4.5: 4.5, weight %;
Whipping agent:
Deionized water;
Linking agent ratio in an embodiment:
Select diethanolamine, trolamine miscellany for use, select diethanolamine: trolamine=1: 2, weight %;
Isocyanic ester numbering in an embodiment:
Isocyanic ester A:TDI80/20 and thick MDI 80: 20, weight %;
Isocyanic ester B:TDI80/20 and thick MDI 50: 50, weight %;
Isocyanic ester C: the remodeling isocyanic ester 2424 of selecting U.S. Huntsman Corporation for use;
Isocyanic ester D: with 20-30 part TM20, the mixture of the thick MDI of 5-15 part and 65-75 part BX118 stirred 1 hour, obtained the isocyanic ester compound according to weight percent, and detect index: NCO content is 36%-40%.Isocyanic ester D is according to above-mentioned three) make.
Below 7 embodiment, the concrete preparation method of polyurethane foam is as follows:
Isocyanic ester in this test is an example with isocyanic ester B
1) in the 300ml stainless steel vessel, add by weight polyether glycol, polymer polyatomic alcohol, water, catalyzer, linking agent and silicone oil successively, and stir with the speed of vertical drill with 1200rpm, be the polyvalent alcohol compound, placed 3 minutes.
2) with in the 300ml stainless steel vessel, weighing 1) 100g polyvalent alcohol compound, according to 100g polyvalent alcohol compound, isocyanate index is 102, calculating and consuming isocyanic ester B quality is 39.2g, so isocyanic ester B add-on is 39.2g, temperature is controlled at 22-23 ℃.
3) with 2) isocyanate component pours 1 into) in the polyvalent alcohol compound, and stir short mix 6-8 second rapidly with the speed of vertical drill with 1200rpm.
4) miscellany is poured in the swage tool of 80mm*80mm*20mm close the cover fast.This mould adopts 50 ℃ of-55 ℃ of hot water circulation control die temperatures, and temperature is at 45 ℃～50 ℃, the demoulding in 4-6 minute.
5) foam sample after the depanning under indoor 20-30 ℃, is placed aging moulding after 24 hours, and censorship is surveyed unit and detected.
In embodiment 1 following table " √ ": the expression present embodiment uses this raw material
| Sequence number | 1-1 | 1-2 | 1-3 | 1-4 |
| Prescription | Weight (g) | Weight (g) | Weight (g) | Weight (g) |
| Polyether glycol 330-1 | 50 | |||
| Polyether glycol 330-2 | 50 | |||
| Polyether glycol 330-3 | 50 | |||
| Polyether glycol 330-4 | 50 | |||
| Polymer polyatomic alcohol 36/28 | 50 | 50 | 50 | 50 |
| Catalyst A | 1.3 | 1.3 | 1.3 | 1.3 |
| Silicone oil A | 0.6 | 0.6 | 0.6 | 0.6 |
| Water | 2.8 | 2.8 | 2.8 | 2.8 |
| Linking agent | 1.0 | 1.0 | 1.0 | 1.0 |
| Isocyanic ester A | √ | √ | √ | √ |
| Isocyanate index | 102 | 102 | 102 | 102 |
| VOC content ppm | 115 | 150 | 112 | 160 |
Among the above embodiment 1 as can be seen: the polyurethane foam VOC content of the urethane raw preparation of using at present is very high, all greater than 100ppm, routine 1-1-1-4 even reach 160ppm.The present invention is from ensuing embodiment comparison test, as can be seen: polyether glycol, polymer polyatomic alcohol, catalyzer, silicone oil and organic isocyanate are one of factors that produces VOC.
Embodiment 2
| Sequence number | 2-1 | 2-2 | 2-3 | 2-4 |
| Prescription | Weight (g) | Weight (g) | Weight (g) | Weight (g) |
| Polyether glycol 330NA-1 | 50 | |||
| Polyether glycol 330NA-2 | 50 | |||
| Polyether glycol 330NA-3 | 50 | |||
| Polyether glycol 330NA-4 | 50 | |||
| Polymer polyatomic alcohol 36/28 | 50 | 50 | 50 | 50 |
| Catalyst A | 1.3 | 1.3 | 1.3 | 1.3 |
| Silicone oil A | 0.6 | 0.6 | 0.6 | 0.6 |
| Water | 2.8 | 2.8 | 2.8 | 2.8 |
| Linking agent | 1.0 | 1.0 | 1.0 | 1.0 |
| Isocyanic ester A | √ | √ | √ | √ |
| Isocyanate index | 102 | 102 | 102 | 102 |
| VOC content ppm | 86 | 101 | 85 | 104 |
From embodiment 2, the polyurethane foam that the 330NA that adopts the present invention to handle prepares can effectively reduce VOC content.Adopt the VOC content of the polyurethane foam of 330NA preparation in the present embodiment 2, the be untreated VOC content of 330N of corresponding embodiment 1 has the bigger range of decrease, the VOC content of comparative example 2-4 and routine 1-4 decreases by 35%, illustrates that the present invention is effective to the processing of 330N.
Embodiment 3
| Sequence number | 3-1 | 3-2 |
| Prescription | Weight (g) | Weight (g) |
| Polyether glycol 330NA-1 | 50 | 50 |
| Polymer polyatomic alcohol 36/28 | 50 | |
| Polymer polyatomic alcohol 36/20 | 50 | |
| Catalyst A | 1.3 | 1.3 |
| Silicone oil A | 0.6 | 0.6 |
| Water | 2.8 | 2.8 |
| Linking agent | 1.0 | 1.0 |
| Isocyanic ester A | √ | √ |
| Isocyanate index | 102 | 102 |
| VOC content ppm | 86 | 42 |
From embodiment 3, polymer polyatomic alcohol has bigger influence to VOC content.VOC content lateral comparison from routine 3-1 and routine 3-2, VOC content decreases by 51%, therefore selects synthetic polymer polyatomic alcohol 36/20 of the present invention, can significantly reduce VOC content in the polyurethane foam.
Embodiment 4
| Sequence number | 4-1 | 4-2 | 4-3 |
| Prescription | Weight (g) | Weight (g) | Weight (g) |
| Polyether glycol 330A-1 | 50 | 50 | 50 |
| Polymer polyatomic alcohol 36/20 | 50 | 50 | 50 |
| Catalyst A | 1.3 | 1.3 | 1.3 |
| Silicone oil A | 0.6 | ||
| Silicone oil B | 0.6 | ||
| Silicone oil C | 0.6 | ||
| Water | 2.8 | 2.8 | 2.8 |
| Linking agent | 1.0 | 1.0 | 1.0 |
| Isocyanic ester A | √ | √ | √ |
| Isocyanate index | 102 | 102 | 102 |
| VOC content ppm | 42 | 38 | 32 |
From embodiment 4, the selection of silicone oil is influential to the VOC content of polyurethane foam, select low atomizing silicone oil, can reduce the VOC content of polyurethane foam, the VOC content of lateral comparison example 4-1 and routine 4-3, the range of decrease is nearly 24%, from routine 4-3 as can be seen the present invention select the German low atomizing silicone oil B8734LF of Gao Shi Mitt USA Corporation certain effect to be arranged to reducing VOC content.
Embodiment 5
| Sequence number | 5-1 | 5-2 | 5-3 | 5-4 |
| Prescription | Weight (g) | Weight (g) | Weight (g) | Weight (g) |
| Polyether glycol 330NA-1 | 50 | 50 | 50 | 50 |
| Polymer polyatomic alcohol 36/20 | 50 | 50 | 50 | 50 |
| Catalyst A | 1.3 | 1.3 | 1.3 | 1.3 |
| Silicone oil C | 0.6 | 0.6 | 0.6 | 0.6 |
| Water | 2.8 | 2.8 | 2.8 | 2.8 |
| Linking agent | 1.0 | 1.0 | 1.0 | 1.0 |
| Isocyanic ester A | √ | |||
| Isocyanic ester B | √ | |||
| Isocyanic ester C | √ | |||
| Isocyanic ester D | √ | |||
| Isocyanate index | 102 | 102 | 102 | 102 |
| VOC content ppm | 32 | 28 | 17 | 18 |
From embodiment 5, the selection of isocyanic ester has bigger influence to VOC content, 5-1 selects isocyanic ester A and 5-2 to select isocyanic ester B, the VOC content of polyurethane foam is higher, 5-3 selects isocyanic ester C and 5-4 to select isocyanic ester D, the VOC content of polyurethane foam has the bigger range of decrease, the maximum range of decrease nearly 47% of lateral comparison VOC content.
Embodiment 6
| Sequence number | 6-1 | 6-2 | 6-3 |
| Prescription | Weight (g) | Weight (g) | Weight (g) |
| Polyether glycol 330NA-1 | 50 | 50 | 50 |
| Polymer polyatomic alcohol 36/20 | 50 | 50 | 50 |
| Catalyst A | 1.3 | ||
| Catalyst B | 0.6 | ||
| Catalyzer C | 1.3 | ||
| Silicone oil C | 0.6 | 0.6 | 0.6 |
| Water | 2.5 | 2.5 | 2.5 |
| Linking agent | 1.0 | 1.0 | 1.0 |
| Isocyanic ester D | √ | √ | √ |
| Isocyanate index | 102 | 102 | 102 |
| VOC content ppm | 19 | 17 | 21 |
From embodiment 6 as can be seen: though the whole standard GB 18586-2001 of VOC content, but catalyst n among the 6-3, the adding of N-dimethylethanolamine, make VOC content rise to some extent, lateral comparison example 6-2 and routine 6-3VOC content, increasing degree is nearly 24%, therefore for reducing VOC content in the polyurethane foam, the this patent suggestion need not or be used N, N-dimethylethanolamine less in selection of catalysts.
Embodiment 7
| Sequence number | 7-1 | 7-2 |
| Prescription | Weight (g) | Weight (g) |
| Polyether glycol 330NA-1 | 50 | 50 |
| Polymer polyatomic alcohol 36/20 | 50 | 50 |
| Catalyst A | 1.3 | 1.3 |
| Silicone oil C | 0.6 | 0.6 |
| Water | 3.1 | 2.8 |
| Linking agent | 1.0 | 1.0 |
| Isocyanic ester C | √ | |
| Isocyanic ester D | √ | |
| Isocyanate index | 102 | 102 |
| Core density g/cm 3 | 49.2 | 48.8 |
| Rebound degree % | 58 | 64 |
| Compressive strength tension set (70 ℃ * 22h, 50%) % | 5.1 | 4.9 |
| Tension fracture elongation rate % | 86 | 119 |
| Tensile strength MPa | 0.165 | 0.264 |
| Tear strength N/cm | 8.8 | 12.8 |
| VOC content ppm | 17 | 19 |
From embodiment 7 as can be seen: routine 7-1 with remodeling MDI and routine 7-2 with isocyanic ester compound of the present invention, all stably the be up to state standards index of GB18586-2001 defined of VOC content.
The polyurethane foam physicals comprises density, rebound degree, tension fracture elongation rate, tensile strength, compressive strength tension set and tear strength.The polyurethane foam that close density is arranged compares rebound degree, tension fracture elongation rate, and tensile strength, compressive strength tension set and tear strength detect data, it is generally acknowledged that the high polyurethane foam of (except the special purpose) test data is better.
From embodiment 7, it can also be seen that: have only that isocyanic ester changes, under other starting material permanence conditions, the detected result of isocyanate foams physicals, be rebound degree, the tension fracture elongation rate among the routine 7-2, these four foam physics performances of tensile strength and tear strength are apparently higher than routine 7-1.Therefore can draw to draw a conclusion: with the physicals of the obtained polyurethane foam of the isocyanic ester compound of the present invention obtained polyurethane foam of MDI that is better than retrofiting.
Conclusion:
Can draw to draw a conclusion from the series of comparisons testing data of embodiment 1 to embodiment 7:
One, the comparison test among embodiment 1, embodiment 2, embodiment 3 and the embodiment 5 as can be seen: obviously influencing polyurethane foam VOC content is polyether glycol, polymer polyatomic alcohol and isocyanic ester.The present invention greatly reduces polyurethane foam VOC content by the optimized choice to the synthetic and isocyanic ester of the processing of polyether glycol, novel polymer polyvalent alcohol.
Two, in the comparison test of embodiment 4 and embodiment 6, catalyzer and silicone oil have certain influence to polyurethane foam VOC content as can be seen, for reducing VOC content in the polyurethane foam better, the silicone oil of the catalyzer of preferred low VOC content and low atomizing.
Three, 7-1 and 7-2 physicals are tested as can be seen in the comparing embodiment: the physicals test data of the prepared polyurethane foam of isocyanic ester compound of the present invention, the physicals test data of MDI obviously is better than retrofiting, therefore to make the physicals of low VOC content polyurethane foam better, should preferred isocyanic ester compound of the present invention.
Claims (10)
1, the preparation method of the polyurethane foam of low volatile organic compound content is characterized in that: raw material is the polyether glycol of handling again, polymer polyatomic alcohol, whipping agent, low smell catalyzer, linking agent, low atomizing silicone oil and the low volatile content isocyanic ester of low volatile content;
The polyvalent alcohol compound comprises polyether glycol, polymer polyatomic alcohol, whipping agent, catalyzer, linking agent and silicone oil;
Polyvalent alcohol compound raw material weight ratio is:
Polyether glycol: 38.1-57.2
Polymer polyatomic alcohol: 37.9-56.1
Whipping agent: 2.5-2.7
Catalyzer: 1.1-1.3
Linking agent: 0.8-1.1
Silicone oil: 0.5-0.7
Ratio is between each raw material: isocyanic ester and polyvalent alcohol compound equivalence ratio are 0.90-1.40, and promptly isocyanate index is 90-140;
The preparation method of polyurethane foam is:
1) in stainless steel vessel A, with polyether glycol, polymer polyatomic alcohol, catalyzer, silicone oil, whipping agent and linking agent, press raw material weight than adding successively, stir, make the polyvalent alcohol compound, placed 3 minutes;
2) in stainless steel vessel B, calculate and weighing isocyanic ester weight according to isocyanate index, to mix, temperature is controlled at 22-23 ℃;
3) take out a certain amount of 1 then) the polyvalent alcohol compound, with 2) isocyanate component pours in the polyvalent alcohol compound, and stirs short mix 6-8 second rapidly;
4) with 3) pour in the swage tool, temperature is controlled at 45 ℃-50 ℃, the demoulding in 4-6 minute;
5) foam sample after the depanning under 20-30 ℃, is placed aging moulding after 24 hours, detects.
2, according to the Preparation Method of the polyurethane foam of claims 1 described low volatile organic compound content, it is characterized in that: the described polyether glycol method of handling again is as follows:
In reactor, by weight percentage, add polyether glycol 330N 96%-98%, finishing agent 0.1%-0.3%, deionized water 1.9%-3.9% is warming up to 80 ℃～90 ℃, stirs 30 minutes, reduced vacuum, temperature is controlled at 105 ℃～110 ℃, and moisture filters discharging less than 0.02-0.04%, promptly get the product that the technology of the present invention is handled, polyether glycol 330NA.
3, according to the preparation method of the polyurethane foam of claims 1 described low volatile organic compound content, it is characterized in that: the polymer polyatomic alcohol method of described low volatile content is as follows:
In reactor, by weight percentage, add polyether glycol 330NA-1 75-85%, trolamine 5-8%, temperature is at 20-50 ℃, and 40-70 adds thick MDI8.5-14% fast in second, add diethanolamine 1.5-3% subsequently, mixed 1-2 hour, temperature is reduced to 30-40 ℃ with bottom discharge, promptly gets low volatile content polymer polyatomic alcohol of the present invention.
4, according to the preparation method of the polyurethane foam of claims 1 described low volatile organic compound content, it is characterized in that: described whipping agent is: deionized water, methylene dichloride, pentane, fluorine Lyons; Preferred deionized water.
5, according to the preparation method of the polyurethane foam of claims 1 described low volatile organic compound content, it is characterized in that: described selection or mixing low volatile content catalyzer are: A-1, A-33, C-225, a kind of or two or more mixtures wherein; Preferred catalyst is: A-1, A-33, the two or more mixtures of C-225.
6, according to the preparation method of the polyurethane foam of claims 1 described low volatile organic compound content, it is characterized in that: described linking agent is: diethanolamine and trolamine.
7, according to the preparation method of the polyurethane foam of claims 1 described low volatile organic compound content, it is characterized in that: the low atomizing of described selection silicone oil is: L-3015, the L-3415 of U.S. Niax company, Y-10366 and German height are executed the B8734LF of German Gao Shi Mitt USA Corporation; Preferred B8734LF.
8, according to the preparation method of the polyurethane foam of claims 1 described low volatile organic compound content, it is characterized in that: described low volatile content isocyanic ester has: TDI80/20, thick MDI, the mixed type isocyanic ester be Japanese NP company's T M20 and remodeling isocyanic ester be Hensel step 2424, the BX118 of Korea S's brocade lake Mitsui.
9, according to the preparation method of the polyurethane foam of claims 8 described low volatile organic compound contents, it is characterized in that: the preparation method of described isocyanic ester compound is: according to weight percent, with 20-30%TM20, the mixture of thick MDI of 5-15% and 65-75%BX118, stirred 1 hour, and be the isocyanic ester compound.
10, by the purposes of the polyurethane foam of claims 1 described low volatile organic compound content, mainly be used in the motor vehicle interior trim, also can be used for indoor sofa, bedding, liner.
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