CN108003318A - A kind of low organic matter release type polyurethane high resilience foam - Google Patents

A kind of low organic matter release type polyurethane high resilience foam Download PDF

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Publication number
CN108003318A
CN108003318A CN201711323942.3A CN201711323942A CN108003318A CN 108003318 A CN108003318 A CN 108003318A CN 201711323942 A CN201711323942 A CN 201711323942A CN 108003318 A CN108003318 A CN 108003318A
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organic matter
cyclodextrin
high resilience
phosphate
release type
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CN108003318B (en
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赵修文
赵卫鸣
张利国
李博
张莉
张涛
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Liming Research Institute of Chemical Industry Co Ltd
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Liming Research Institute of Chemical Industry Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666—Compounds of group C08G18/48 or C08G18/52
    • C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
    • C08G18/6688—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3271
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0009—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Glucans, e.g. polydextrose, alternan, glycogen; (alpha-1,4)(alpha-1,6)-D-Glucans; (alpha-1,3)(alpha-1,4)-D-Glucans, e.g. isolichenan or nigeran; (alpha-1,4)-D-Glucans; (alpha-1,3)-D-Glucans, e.g. pseudonigeran; Derivatives thereof
    • C08B37/0012—Cyclodextrin [CD], e.g. cycle with 6 units (alpha), with 7 units (beta) and with 8 units (gamma), large-ring cyclodextrin or cycloamylose with 9 units or more; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3271—Hydroxyamines
    • C08G18/3275—Hydroxyamines containing two hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4804—Two or more polyethers of different physical or chemical nature
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/125—Water, e.g. hydrated salts
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2110/00—Foam properties
    • C08G2110/0083—Foam properties prepared using water as the sole blowing agent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/10—Water or water-releasing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • C08J2375/08—Polyurethanes from polyethers

Abstract

The invention discloses a kind of low organic matter release type polyurethane high resilience foam, it is characterized in that being added with phosphate cyclodextrin in raw material, the phosphate cyclodextrin is made by following methods：(1) it is phosphate and urea is soluble in water, it is uniformly mixed, is 5.0~6.0 with acid-conditioning solution pH value；(2) cyclodextrin is added in above-mentioned mixed solution, is filtered after stirring evenly, filtration cakes torrefaction to moisture is less than 12% mass parts, and grinding, then keeps 5h under the conditions of 150 ± 5 DEG C；(3) it is washed with water, filters, is dry, up to phosphate cyclodextrin.In terms of polyether polyol in polyurethane high resilience foam raw material and polymer polyatomic alcohol gross mass, phosphate cyclodextrin recommends additive amount as 1% 5% mass parts.

Description

A kind of low organic matter release type polyurethane high resilience foam
Technical field
The present invention relates to polyurethane high resilience foam preparation, and in particular to low organic matter release type polyurethane high resilience foam And preparation method thereof.
Background technology
Polyurethane high resilience foam is a kind of mat material of high comprehensive performance, is widely used in automotive seat and furniture etc.. The high rebound foam of conventional urethane can slowly discharge volatile organic matter in use, as benzene homologues, aldoketones, amine, Nitrile and small molecule organosilicon etc..These poisonous and harmful volatile organic matters can rapidly result in surrounding enviroment deterioration.In addition, such High rebound foam is chiefly used in automobile or confined space, the gas such as interior should not be spread, and extended stationary periods in the environment will be serious The health of foam user is damaged, environmental degradation also can be more serious.
Patent document WO2005118668A1 discloses a kind of method for reducing the volatile organic matter as caused by silicone oil, should Method introduces hydroxyl by the end group in silicone oil, silicone oil is bonded in PU body structure, effectively reduces small point The volatilization of sub- silicone oil.
Patent document CN101240055A discloses a kind of preparation method of low VOC content polyurethane foam, and this method is led to Cross and processing early period is carried out to raw material polyether polyol, specifically heated, stirred and taken out under refining agent, deionized water auxiliary Vacuum, further to feed purification, to reduce wherein volatile organic matter.
Patent document US2010174006A1 discloses a kind of method for reducing polyurethane foam volatile organic matter, the party Method reduces the release of volatile organic matter by adding activated carbon, zeolite etc. in the preparation process of polyurethane foam, but living Property charcoal can make polyurethane foam blackening, it is difficult to popularize in an all-round way, in addition zeolite can to polyurethane high resilience foam prepare technique bar Part produces considerable influence, and the especially metering pump infringement to high pressure foaming machine is larger.
It is higher that prior art unsatisfactorily solves polyurethane high resilience foam release volatile organic matter This technical problem.
The content of the invention
The object of the present invention is to provide a kind of low organic matter release type polyurethane high resilience foam.
The technical scheme is that phosphate cyclodextrin, the phosphate ring are added in polyurethane high resilience foam raw material Dextrin is made by following methods：
(1) it is phosphate and urea is soluble in water, it is uniformly mixed, is 5.0~6.0 with acid-conditioning solution pH value.One As stir 20~30min.
(2) cyclodextrin is added in above-mentioned mixed solution, is filtered after stirring evenly, filtration cakes torrefaction to moisture is less than 12% matter Part is measured, grinding, then keeps 5h under the conditions of 150 ± 5 DEG C.
(3) it is washed with water, filters, is dry, up to phosphate cyclodextrin.
The preferable stirring condition of step (1) is 20~30min of stirring under 35 ± 5 DEG C of water-baths.
Step (2) filter cake is preferably dried in vacuo under the conditions of 50~60 DEG C.
The phosphate includes orthophosphates or polyphosphate, such as Na2HPO4、NaH2PO4, tripolyphosphate, six poly- phosphorus Hydrochlorate, trimetaphosphate or hexametaphosphate etc..
The cyclodextrin includes alpha-cyclodextrin, beta-cyclodextrin or gamma-cyclodextrin and its derivative or its mixture.
In terms of polyether polyol in polyurethane high resilience foam raw material and polymer polyatomic alcohol gross mass, phosphate cyclodextrin Recommendation additive amount is 1%-5% mass parts.
Phosphate cyclodextrin of the present invention is added suitable for polyurethane foam combination, can reduce gained foam Volatile organic matter discharges, and is particularly stabilized in polyurethane high resilience foam composition polyol component, in 6 months not Generation retrogradation phenomenon, does not produce harmful effect, not to the mechanical property and anti-flammability of foam to the preparation process of high rebound foam Harmful effect can be produced.
The present invention provides a kind of low organic matter release type polyurethane high resilience foam, and raw material is made of two component of A, B, by matter Amount part meter includes：
Component A (polyol component)：Including 100~50 parts of polyether polyol, 0~50 part of polymer polyatomic alcohol；Catalyst 0.2~5 part；1~5 part of foaming agent；Foam stabiliser 0.2~3；0.2~6 part of crosslinking agent；1~5 part of phosphate cyclodextrin；Wherein Polyether polyol is 100 parts with polymer polyatomic alcohol total amount；
B component (polyisocyanate component)：Including TDI, MDI, polymeric MDI or modified MDI etc. and its mixture.
A/B mass ratioes are 100: 30~100: 80.
Preferable polyether polyols alcohol functionalities are 3, and relative molecular mass is 4700~8000, proportion of primary OH groups in terminal hydroxy group More than 70%.
The graft copolymer of the polymer polyatomic alcohol preferred, polyethers polyalcohol and styrene-acrylonitrile.
The preferred response type amine of catalyst；The preferred deionized water of foaming agent；The foam stabiliser is preferably poly- Silicone-polyether copolymer；The preferred alcamine compound of crosslinking agent.
Inventive formulation is reasonable, prepared low organic matter release type polyurethane high resilience foam and the high rebound foam of tradition Compare, have the characteristics that organic matter burst size is extremely low, conventional urethane high-resilience foam material organic matter burst size mistake can be improved The defects of high.
The method for preparing low organic matter release type polyurethane high resilience foam, comprises the following steps：(1) by polyether polyols Alcohol, polymer polyatomic alcohol, catalyst, foaming agent, foam stabiliser, crosslinking agent and phosphate cyclodextrin are mixed and disperseed by metering Uniform to obtain component A, polyisocyanates is B component；(2)：Component A and B component is abundant by 100: 30~100: 80 mass ratio It is uniformly mixed and injects in the mould that mould temperature is 40~80 DEG C, 2~10min of curing returns up to low organic matter release type polyurethane is high Play foamed material.
Embodiment
The present invention is described in further detail with comparative example with reference to embodiment.
The preparation of phosphate cyclodextrin：By 45g orthophosphates (Na2HPO4·12H2O：NaH2PO4·2H2The amount ratio of O materials 3: 1) be dissolved in 4g urea in 100mL water, and stir 20min under 35 ± 5 DEG C of water-baths and be uniformly mixed, solution is adjusted with dilute sulfuric acid PH value is 5.5；100g beta-cyclodextrins are added into above-mentioned mixed solution, continues to stir 30min, filters, filter cake is under the conditions of 55 DEG C It is 10% to be dried under vacuum to moisture, and grinding is uniform, then keeps 5h under the conditions of 150 DEG C；After, it is placed in suction funnel, 10mL water wash is used during suction filtration respectively 3 times；It is dried in vacuo under the conditions of 45 DEG C, crushed 200 mesh sieves, up to phosphate ring Dextrin.
The method that embodiment prepares polyurethane high resilience foam with comparative example is as follows：
(1)：By polyether polyol, polymer polyatomic alcohol, catalyst, foaming agent, foam stabiliser, crosslinking agent, phosphate Cyclodextrin mass parts as shown in table 1 are added in container, are thoroughly mixed and are uniformly dispersed, obtain component A；
Wherein polyether polyol for can Leah polyalcohol (Nanjing) Co., Ltd KPX KE-810, polymer polyatomic alcohol is Can Leah polyalcohol (Nanjing) Co., Ltd KPX KE-8080S, catalyst be Mitugao New Material Group Niax EF- 700, foaming agent is deionized water, and foam stabiliser selects the DC2525 of U.S.'s Air Products Company, crosslinking agent for Yangtze petrochemical industry- The diethanol amine of BASF Co., Ltd.
Each material quality number in 1 component A of table
Raw material Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Comparative example
Polyether polyol 100 100 100 50 100
Polymer polyatomic alcohol 0 0 0 50 0
Catalyst 1.0 1.0 1.0 1.0 1.0
Foaming agent 3.5 3.5 3.5 3.5 3.5
Foam stabiliser 0.8 0.8 0.8 0.8 0.8
Crosslinking agent 0.6 0.6 0.6 0.6 0.6
Phosphate cyclodextrin 5 3 1 1 0
B component is the Wannate 8018 of Yantai Wanhua Polyurethane Co., Ltd.
(2)：Component A obtained by (1) and B component in mass ratio 100: 55 are sufficiently mixed uniformly and are uniformly injected into mould temperature as 60 In DEG C mould, 5min is up to polyurethane high resilience foam for curing, and core density is 55kg/m3。
Naturally volatile organic matter test is carried out to prepared polyurethane high resilience foam after curing 24h.Test method is Pocket type method, using 10L sampler bags, sample temperature is 65 DEG C, and volatile organic matter sampling quantity is 1.0L, and aldoketones sampling quantity is 2.0L.Test result is shown in Table 2.
2 volatile organic matter test result of table
Remarks：Unit is μ g/m3, TVOC is volatile organic matter total amount, and N.D., which represents not detect, (to be less than method to detect Limit), aldoketones detection is limited to 50 μ g/m3, the detection of indivedual volatile organic matters is limited to 10 μ g/m3, TVOC detection be limited to 100 μ g/ m3。
From testing result, benzene class, the burst size of aldehydes volatile organic matter significantly reduce in material of the present invention, TVOC decreases by 47% compared with prior art material burst size, the total burst size very little of material volatile organic matter.

Claims (10)

  1. A kind of 1. low organic matter release type polyurethane high resilience foam, it is characterized in that being added with phosphate cyclodextrin, institute in raw material Phosphate cyclodextrin is stated to be made by following methods：
    (1) it is phosphate and urea is soluble in water, it is uniformly mixed, is 5.0~6.0 with acid-conditioning solution pH value；
    (2) cyclodextrin is added in above-mentioned mixed solution, is filtered after stirring evenly, filtration cakes torrefaction to moisture is less than 12% mass Part, grinding, then keeps 5h under the conditions of 150 ± 5 DEG C；
    (3) it is washed with water, filters, is dry, up to phosphate cyclodextrin.
  2. 2. low organic matter release type polyurethane high resilience foam according to claim 1, it is characterized in that step (1) stirring bar Part is 20~30min of stirring under 35 ± 5 DEG C of water-baths；Step (2) filter cake is dried in vacuo under the conditions of 50~60 DEG C.
  3. 3. low organic matter release type polyurethane high resilience foam according to claim 1, the phosphate refer to orthophosphoric acid Salt or polyphosphate.
  4. 4. low organic matter release type polyurethane high resilience foam according to claim 3, the phosphate refer to Na2HPO4、 NaH2PO4, tripolyphosphate, six Quadrafos, trimetaphosphate or hexametaphosphate.
  5. 5. low organic matter release type polyurethane high resilience foam according to claim 1, the cyclodextrin refers to α-ring paste Essence, beta-cyclodextrin or gamma-cyclodextrin and its derivative or its mixture.
  6. 6. low organic matter release type polyurethane high resilience foam according to claim 1, it is characterized in that：Returned so that polyurethane is high Polyether polyol and polymer polyatomic alcohol gross mass meter in foam raw material are played, it is 1%-5% that phosphate cyclodextrin, which recommends additive amount, Mass parts.
  7. 7. low organic matter release type polyurethane high resilience foam according to claims 1 to 6, raw material is by two component group of A, B Into including in parts by mass：
    Component A (polyol component)：Including 50~100 parts of polyether polyol, 0~50 part of polymer polyatomic alcohol；Catalyst 0.2~ 5 parts；1~5 part of foaming agent；Foam stabiliser 0.2~3；0.2~6 part of crosslinking agent；1~5 part of phosphate cyclodextrin；Wherein polyethers Polyalcohol is 100 parts with polymer polyatomic alcohol total amount；
    B component (polyisocyanate component)：Including TDI, MDI, polymeric MDI or modified MDI and its mixture；
    A/B mass ratioes are 100: 30~100: 80.
  8. 8. low organic matter release type polyurethane high resilience foam according to claim 7, polyether polyols alcohol functionalities are 3, Relative molecular mass is 4700~8000, and proportion of primary OH groups is more than 70% in terminal hydroxy group.
  9. 9. low organic matter release type polyurethane high resilience foam according to claim 7, the polymer polyatomic alcohol is poly- The graft copolymer of ethoxylated polyhydric alcohol and styrene-acrylonitrile.
  10. 10. low organic matter release type polyurethane high resilience foam according to claim 6, the catalyst is response type amine Class；The foaming agent is deionized water；The foam stabiliser is polysiloxane polyether copolymer；The crosslinking agent is alcamines Compound.
CN201711323942.3A 2017-11-30 2017-11-30 Low-organic-matter-release polyurethane high-resilience foam Active CN108003318B (en)

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Publication number Priority date Publication date Assignee Title
CN109553742A (en) * 2018-12-06 2019-04-02 上海应用技术大学 A kind of manufacture craft of low VOC polyurethane automobile seat

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