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CN100497430C - Method of preparing full MDI polyurethane slow rebound foam - Google Patents

Method of preparing full MDI polyurethane slow rebound foam Download PDF

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CN100497430C
CN100497430C CNB2006100707111A CN200610070711A CN100497430C CN 100497430 C CN100497430 C CN 100497430C CN B2006100707111 A CNB2006100707111 A CN B2006100707111A CN 200610070711 A CN200610070711 A CN 200610070711A CN 100497430 C CN100497430 C CN 100497430C
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polyol
foam
mdi
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functionality
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CN101016368A (en
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张谦和
喻建明
刘新建
林芳茜
崔能伟
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Wanhua Chemical Group Co Ltd
Wanhua Chemical Beijing Co Ltd
Wanhua Chemical Guangdong Co Ltd
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Yantai Wanhua Polyurethanes Co Ltd
Beijing Keju Chemical New Material Co Ltd
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Abstract

本发明涉及一种全MDI聚氨酯慢回弹泡沫的制备方法，属于聚氨酯泡沫制备技术领域。全MDI聚氨酯慢回弹泡沫的制备方法，特征在于原料组成包括如下的组分：a.MDI体系异氰酸酯，官能度是2.1～2.5；b.聚醚多元醇组分；c.发泡剂；d.催化剂、表面活性剂。本发明的全MDI聚氨酯慢回弹泡沫的制备方法，组合聚醚中包括大宗聚醚产品和相关助剂，不含物理发泡剂，可以稳定存放；异氰酸酯组分包括MDI及其预聚体，不包含TDI，所制备的慢回弹泡沫50%的永久性变小于10%，所制备的泡沫适用于枕芯、腰垫、床垫等家居用品。The invention relates to a method for preparing an all-MDI polyurethane slow-rebound foam, and belongs to the technical field of polyurethane foam preparation. The preparation method of all MDI polyurethane slow resilience foam is characterized in that the raw material composition includes the following components: a. MDI system isocyanate, the functionality is 2.1 to 2.5; b. polyether polyol component; c. foaming agent; d. . Catalyst, surfactant. The preparation method of the all-MDI polyurethane slow-rebound foam of the present invention includes bulk polyether products and related auxiliary agents in the combined polyether, does not contain a physical foaming agent, and can be stored stably; the isocyanate component includes MDI and its prepolymer, Does not contain TDI, the permanent change of 50% of the prepared slow rebound foam is less than 10%, and the prepared foam is suitable for pillow cores, waist pads, mattresses and other household products.

Description

The preparation method of all-MDI polyurethane low resilience urethane foam resilient foam
Technical field
The present invention relates to a kind of preparation method of all-MDI polyurethane low resilience urethane foam resilient foam, belong to the polyurethane foam preparing technical field.
Background technology
As everyone knows, polyurethane low resilience urethane foam resilient foam is referred to as memory foam, viscoelastic foam, and its unique distinction is the shape that can comply with carrier, makes contact area maximization, stress gradient minimize, stressed centrostigma can be eased, local not extruding and sensation of pricking.Therefore, low resilience urethane foam resilient foam is widely used as pillow, mattress, cushion etc., helps the blood of human body circulation, is a kind of high-comfort health care foam.
MDI, TDI or its miscellany all can be used to prepare low resilience urethane foam resilient foam, and MDI is having certain advantage than TDI aspect the Technology, and MDI reactive behavior height can reduce catalyst levels, thereby has reduced foamy VOC; MDI has the index range of relative broad, can regulate foamy hardness and rebound resilience by changing index in this scope.In addition, MDI also has environment-friendly advantage than TDI, helps the healthy of site operation personnel.
The rebound resilience of polyurethane foam is relevant with second-order transition temperature with its degree that is separated in theory, by selecting raw material the foamy second-order transition temperature is adjusted to use temperature, reduces the foamy degree that is separated simultaneously, can obtain low resilience urethane foam resilient foam.Common operational path is the polyethers of soft bubble polyethers of low hydroxyl value and higher hydroxyl value to be mixed use, and improves the foamy cross-linking density, thereby has both improved the foamy second-order transition temperature, has reduced the degree of being separated again.All be based on this theory as CN1606580, CN1572186, CN1229803.But this method closed pore problem in preparation low resilience urethane foam resilient foam process is common, makes that moulded foam side when opening mould is easy to crack, also can cause foam contraction, has influence on foamy outward appearance and yield rate.Adding pore-creating agent is the common means that solve the closed pore problem, but commercially available pore-creating agent costs an arm and a leg, and has increased raw materials cost, and effect sometimes neither be very good, also is a factor that causes combined polyether not stablize depositing.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, the preparation method of the all-MDI polyurethane low resilience urethane foam resilient foam that deposit, the reaction system perforate that provides a kind of combined polyether to stablize.
The preparation method of all-MDI polyurethane low resilience urethane foam resilient foam of the present invention, special character is that the raw material composition comprises following component:
A.MDI system isocyanate, functionality are 2.1～2.5;
B. polyether polyatomic alcohol component;
C. whipping agent;
D. catalyzer, tensio-active agent.
Described isocyanate component comprises MDI, performed polymer and the oligopolymer of different isomerization body;
Described polyether glycol is to be catalyzer with potassium hydroxide, or be catalyzer with double metal cyanide (DMC), with propylene glycol or glycerine or TriMethylolPropane(TMP) small molecules polyvalent alcohol is initiator, with propylene oxide or oxyethane or its miscellany is polymerization single polymerization monomer, ring-opening polymerization forms, and the propylene oxide block structure different with oxyethane directly influences the performance of polyether glycol.
In addition, described polyether glycol also can be the vinyl polymer grafted polyether polyol, be referred to as polyether (POP), also be applicable to reaction system of the present invention, polyether POP is to be basic polyethers with general polyether glycol, unsaturated vinyl monomers such as vinylbenzene, vinyl cyanide, methyl methacrylate, vinyl acetate carry out radical polymerization and form under action of evocating, these free radical polyalcohols stably are present in the basic polyethers with the form of solid particulate; Polyether POP can improve the foamy bearing capacity, also has certain perforate effect simultaneously.
Described polyether glycol has following constitutional features:
The polyol of polyol A propylene oxide, oxyethane, the random or end-blocking copolymerization of oxyethane, EO content is 10～20%, functionality is 3, hydroxyl value 24～56mg KOH/g;
The polyol of polyol B propylene oxide, oxyethane, EO content be less than 10%, and functionality is less than 3, hydroxyl value 28～112mg KOH/g;
The polyol of polyol C propylene oxide, oxyethane, EO content are less than 10%, and functionality is 3～4, hydroxyl value 168～420mg KOH/g;
The polyol of polyol D propylene oxide, oxyethane, EO content it is desirable to greater than 70% greater than 50%, and functionality is 3, hydroxyl value 35～56mg KOH/g;
The polyol of polyol E propylene oxide, oxyethane, EO content it is desirable to 70～100% greater than 50%, and functionality is 3, hydroxyl value 112～240mg KOH/g;
The part by weight that various polyvalent alcohols account for whole polyether glycol total amount is that the weight content of polyolA 30～50%, polyolB5～10%, polyol C40～60%, polyol D+polyol E is 5～10%, and the ratio of polyolD/polyol E weight content is 0.14～0.35.
Preparation polyurethane foam whipping agent commonly used goes for the present invention, as H 2O, 141b, pentane, methylene dichloride etc., these whipping agents can be used alone or as a mixture.Because low resilience urethane foam resilient foam is used for household articles more, the general residual bigger smell of pneumatogen does not advise using pneumatogen.H among the present invention 2O is single whipping agent, does not add any physics auxiliary blowing agent; Consumption is with respect to 1～3% of 100 parts of admixtured polyethers, according to the requirement to foam density, can suitably increase and decrease H 2The content of O.
Described tensio-active agent is the common soft bubble of preparation urethane and the tensio-active agent of high resilience, product has TEGOSTAB B8002, B8715LV, NIAX L-3002, NIAX L-580, NIAX L-5309, DC2585 etc., it also can be other products, size according to material viscosity, reactive behavior, select the strong and weak different tensio-active agent of steady bubble effect, consumption generally is the weight ratio 0.5～1.0% of relative polyether glycol total amount.
In the polyurethane foam production process, have the chemical reaction of many complexity, catalyzer is very important auxiliary agent, is used for reaction speed, makes foaming and gel reaction reach balance.So-called foamable reaction is exactly active group-NCO and the H in the isocyanic ester 2O generated reactive gas carbonic acid gas makes the process of foam expansion; Gel reaction is the reaction of the active group-OH of active group-NCO in the isocyanic ester and polyvalent alcohol, makes the abscess network reach the process of sufficient intensity.The kind of this field useful catalyst is a lot, as two (dimethylamino ethyl) ether, five methyl diethylentriamine, N, N '-dimethylcyclohexylamine, triethylene diamine, stannous octoate, dibutyl tin laurate and retardance catalyzer etc., selecting wherein, one or more mix use; Preferred amines catalyst and delaying type catalyzer thereof.
Also can use chainextender and linking agent in the preparation of low resilience urethane foam resilient foam.
Chainextender generally is the small molecules polyvalent alcohol or the aminated compounds of two functionality, as ethylene glycol, Diethylene Glycol, triethylene glycol, propylene glycol, dipropylene glycol, tripropylene glycol, butyleneglycol, low-molecular-weight PPG, 3,5-diethyl toluene diamine (DETDA), 3,5-diformazan sulfenyl tolylene diamine (DMTDA), 4,4 '-two Zhong Ding ADP methylmethanes (DBMDA).Because the index of low resilience urethane foam resilient foam is lower, degree of crosslinking is higher, use chainextender can improve the foamy tensile strength, consumption generally is the weight ratio 0.3～1.0% of relative polyether glycol total amount.
Linking agent is a functionality greater than 2 small molecules polyvalent alcohol or aminated compounds, as glycerine, diethanolamine, trolamine etc.Preferred alcohols amine linking agent except that the effect of playing the abscess network cross-linked, also can play katalysis when preparing more low-density low resilience urethane foam resilient foam, the speed of balance foaming and gel, and consumption generally is the weight ratio 0.5～1.5% of relative polyether glycol total amount.
Among the low resilience urethane foam resilient foam preparation method of the present invention, except whipping agent, tensio-active agent, catalyzer, chainextender, linking agent, also can add needed other complementary additive, as fire retardant, oxidation inhibitor, mould inhibitor, tinting material, mineral filler etc.Low resilience urethane foam resilient foam is mainly used in household articles, and there is strict requirement in some country to flame retardant resistance, and corresponding standard is also arranged, as the CAL117A of the U.S., DIN75200, the BS5852 of Britain etc. of Germany.Fire retardant is very important a kind of additive in the polyurethane foam, production firm also constantly releases BACN, as the additive flame retardant FM-550 of Chemtura company, the additive flame retardant V6-LS and the reactive flame retardant RX-35 of Albemarle company, also has the solid flame retardant trimeric cyanamide, the degree of scatter of trimeric cyanamide in polyethers has bigger influence to its flame retardant effect, mixes with liquid flame retardant to use to reach better flame retardant effect.
All MDI in the isocyanate component described in the present invention, here the meaning of " all MDI " is not contain TDI, comprise 4,4 '-MDI, 2,4 '-MDI, 2,2 '-MDI, MDI performed polymer and oligopolymer, the NCO content of mixture is 26～30%, preferred 26.5～29%, functionality is 2.1～2.3.
Low resilience urethane foam resilient foam of the present invention is to form through isocyanate component and the reaction of polyol component thorough mixing, adopt low press or high-pressure unit, prepare moulded foam or piece bubble, different with regular foam is that index of Response is lower, the index of Response here is meant the ratio of the equivalents of isocyanate groups NCO and its active hydrogen, be generally less than 80%, the NCO active hydrogen is excessive in reaction system.The slow rebound resilience of foamy was obvious when index was low, but index makes foamy resistance to fatigue, mechanical property relatively poor again when too low, and suitable index of Response of the present invention is 70～80%;
Polyethers, whipping agent, tensio-active agent, catalyzer are joined in the plastic beaker, after stirring, get a part and in test tube, leave standstill, observe stable case; 24～28 ℃ of temperature of charge in the maintenance beaker, and then adding modification MDI24～28 ℃, stir after 5～8 seconds, pour into rapidly in the aluminium matter mould, keep 48-52 ℃ of mould temperature, the demoulding in 6～7 fens, the about 75kg/m of the density of molding sample 3
Expect temperature control at 24～28 ℃, isocyanic ester flow 80～100g/s, polyvalent alcohol flow 160～180g/s; The heating of mould thermostatical circulating water, the about 48-52 of die temperature ℃, after mixture injects mould, 6～7min demoulding.
The ratio of the raw material that relates among the present invention is all by weight calculating, special dated except.
The preparation method of all-MDI polyurethane low resilience urethane foam resilient foam of the present invention comprises large polyether product and relevant auxiliary agent in the combined polyether, do not contain pneumatogen, can stablize and deposit; Isocyanate component comprises MDI and performed polymer thereof, does not comprise TDI, and the permanent of prepared low resilience urethane foam resilient foam 50% diminishes in 10%, and prepared foam is applicable to household articles such as pillow, bustle, mattress.
Embodiment
Polyol 1 is initial by glycerine, propylene oxide, ethylene oxide-capped polyol, and functionality is 3, EO content 14%, hydroxyl value 35mg KOH/g;
Polyol 2 is initial by glycerine, propylene oxide, oxyethane random copolymerization polyvalent alcohol, and functionality is 3, EO content 13%, hydroxyl value 24mg KOH/g;
Polyol 3 propylene glycol are initial, the propylene oxide polymerized polyalcohol, and functionality is 2, PO content 100%, hydroxyl value 56mg KOH/g;
Polyol 4 vinylbenzene, acrylonitrile compolymer graft modification polyether glycol, solid content 30%, hydroxyl value 24mg KOH/g;
Polyol 5 propylene oxide ring-opening polymerization polyvalent alcohols, functionality is 3, PO content 100%, hydroxyl value 240mg KOH/g.
The polyol of polyol 6 propylene oxide, oxyethane, EO content 73%, functionality is 3, hydroxyl value 42mg KOH/g;
The polyol of polyol 7 propylene oxide, oxyethane, EO content 100%, functionality is 3, hydroxyl value 168mgKOH/g;
H 2The O whipping agent
L-3002 tensio-active agent, GE product
B8715LV tensio-active agent, Degussa product
B8002 tensio-active agent, Degussa product
DC5169 tensio-active agent, Air Product product
The conventional kicker of A1
The conventional gel catalyst of A33
DC8154 delayed gel catalyzer, Air Product product
The DEOA diethanolamine
The DEG Diethylene Glycol
Isocyanate modification MDI, the 60%th, MDI, the 40%th, the performed polymer of MDI and oligopolymer, NCO content is 27.3%;
Following Example is to further instruction of the present invention, but authority of the present invention not merely is confined in following several examples, and the person skilled in art is very clear, and any change on the example basis can not left aim of the present invention.
The operation steps of embodiment is that polyethers, water, silicone oil, catalyzer etc. are joined in the plastic beaker in the ratio that designs, and stirs after (being generally 30 seconds) with electric mixer, gets a part and leave standstill, observe stable case in test tube; Keep 24～28 ℃ of temperature of charge in the beaker, and then add the modification MDI (24～28 ℃) of requirement as early as possible, stir after 5～8 seconds, pour into rapidly in the aluminium matter mould, 200 * 200 * 100mm keeps 50 ℃ of mould temperature, the demoulding in 6～7 fens, the about 75kg/m of the density of molding sample 3Sample is deposited test data after 72 hours at normal temperatures.
Industrial equipments is to adopt the low pressure foaming machine, expects temperature control at 24～28 ℃, isocyanic ester flow 80～100g/s, polyvalent alcohol flow 160～180g/s; Aluminium matter industry pillow mould, the thermostatical circulating water heating; About 50 ℃ of die temperature, after mixture injects mould, 6～7min demoulding, the about 75kg/m of the density of finished product pillow 3
Table 1. invention example
*" stablize " feeling the pulse with the finger-tip and do not detect foam local dent, distortion
*" stablize " and refer under the normal temperature that range estimation is less than layering in 4 weeks, " instability " refers to estimate layering in 2 days
Table 2. comparative example
Figure C200610070711D00092
Figure C200610070711D00101
*" stablize " feeling the pulse with the finger-tip and do not detect foam local dent, distortion, " contraction " refers to obviously to estimate smaller volume
*" stablize " and refer under the normal temperature that range estimation is less than layering in 4 weeks, " instability " refers to estimate layering in 2 days
Table 3. example foamy of the present invention rerum natura
Figure C200610070711D00102

Claims (6)

1、全MDI聚氨酯慢回弹泡沫的制备方法，原料组成包括如下的组分：1. The preparation method of all-MDI polyurethane slow rebound foam, the raw material composition includes the following components: a.MDI体系异氰酸酯，官能度是2.1～2.5；a. MDI system isocyanate, the functionality is 2.1-2.5; b.聚醚多元醇；b. polyether polyol; c.发泡剂；c. Foaming agent; d.催化剂和表面活性剂；d. Catalysts and surfactants; 特征在于，所述的聚醚多元醇具有如下的结构特征：It is characterized in that described polyether polyol has the following structural features: polyol A环氧丙烷、环氧乙烷的共聚多元醇，环氧乙烷无规或封端共聚，EO含量是10～20％，官能度是3，羟值24～56mg KOH/g；Polyol A is a copolymerized polyol of propylene oxide and ethylene oxide, random or end-capped copolymerization of ethylene oxide, the EO content is 10-20%, the functionality is 3, and the hydroxyl value is 24-56 mg KOH/g; polyol B环氧丙烷、环氧乙烷的共聚多元醇，EO含量小于10％，官能度小于3，羟值28～112mg KOH/g；Polyol B is a copolymerized polyol of propylene oxide and ethylene oxide, with an EO content of less than 10%, a functionality of less than 3, and a hydroxyl value of 28-112 mg KOH/g; polyol C环氧丙烷、环氧乙烷的共聚多元醇，EO含量小于10％，官能度是3～4，羟值168～420mg KOH/g；Polyol C is a copolymerized polyol of propylene oxide and ethylene oxide, with an EO content of less than 10%, a functionality of 3 to 4, and a hydroxyl value of 168 to 420 mg KOH/g; polyol D环氧丙烷、环氧乙烷的共聚多元醇，EO含量大于50％，官能度是3，羟值35～56mg KOH/g；polyol D is a copolymerized polyol of propylene oxide and ethylene oxide, with an EO content greater than 50%, a functionality of 3, and a hydroxyl value of 35-56 mg KOH/g; polyol E环氧丙烷、环氧乙烷的共聚多元醇，EO含量大于50％，官能度是3，羟值112～240mg KOH/g；Polyol E is a copolymerized polyol of propylene oxide and ethylene oxide, with an EO content greater than 50%, a functionality of 3, and a hydroxyl value of 112-240 mg KOH/g; 各种多元醇相对聚醚多元醇总量的重量比例是polyol A 30～50％、polyol B5～10％、polyol C40～60％、polyol D+polyol E的重量含量是5～10％，polyolD/polyol E重量含量的比值是0.14～0.35。The weight ratio of various polyols relative to the total amount of polyether polyols is polyol A 30-50%, polyol B 5-10%, polyol C 40-60%, polyol D+polyol E weight content is 5-10%, polyol D/ The ratio of polyol E weight content is 0.14～0.35. 2、按照权利要求1所述全MDI聚氨酯慢回弹泡沫的制备方法，特征在于发泡剂为H2O、戊烷、二氯甲烷中的一种或几种，用量为相对于100份聚醚多元醇的重量比1～3％。2. According to the preparation method of the all-MDI polyurethane slow-rebound foam according to claim 1, it is characterized in that the blowing agent is one or more of H 2 O, pentane, and methylene chloride, and the consumption is relative to 100 parts polystyrene The weight ratio of ether polyol is 1-3%. 3、按照权利要求1所述全MDI聚氨酯慢回弹泡沫的制备方法，特征在于所述表面活性剂为制备聚氨酯的普通软泡和高回弹的表面活性剂，用量为相对聚醚多元醇总量的重量比0.5～1.0％。3, according to the preparation method of the described all-MDI polyurethane slow resilience foam of claim 1, it is characterized in that described tensio-active agent is the tensio-active agent of common soft foam and high resilience of preparing polyurethane, and consumption is relative polyether polyol total The weight ratio of the amount is 0.5-1.0%. 4、按照权利要求1所述全MDI聚氨酯慢回弹泡沫的制备方法，特征在于催化剂为双(二甲胺基乙基)醚、五甲基二亚乙基三胺、N，N’-二甲基环己胺、三乙烯二胺、辛酸亚锡、二月桂酸二丁基锡，选择其中一种或几种混合使用。4. According to the preparation method of the all-MDI polyurethane slow-rebound foam according to claim 1, it is characterized in that the catalyst is bis(dimethylaminoethyl)ether, pentamethyldiethylenetriamine, N,N'-di Methylcyclohexylamine, triethylenediamine, stannous octoate, dibutyltin dilaurate, choose one of them or mix them. 5、按照权利要求1所述全MDI聚氨酯慢回弹泡沫的制备方法，特征在于慢回弹泡沫的制备中还使用扩链剂和交联剂，扩链剂是两个官能度的小分子多元醇或胺类化合物，用量是相对聚醚多元醇总量的重量比0.3～1.0％；交联剂是官能度大于2的小分子多元醇或胺类化合物，用量是相对聚醚多元醇总量的重量比0.5～1.5％。5. According to the preparation method of the all-MDI polyurethane slow-rebound foam according to claim 1, it is characterized in that a chain extender and a cross-linking agent are also used in the preparation of the slow-rebound foam, and the chain extender is a small molecule multi-component compound with two functionalities. Alcohol or amine compound, the amount used is 0.3-1.0% by weight relative to the total amount of polyether polyol; the crosslinking agent is a small molecular polyol or amine compound with a functionality greater than 2, and the amount used is relative to the total amount of polyether polyol The weight ratio of 0.5 ~ 1.5%. 6、按照权利要求1所述全MDI聚氨酯慢回弹泡沫的制备方法，特征在于6, according to the preparation method of the all-MDI polyurethane slow rebound foam described in claim 1, it is characterized in that 慢回弹泡沫是经MDI体系异氰酸酯和聚醚多元醇充分混合反应而成，采用低压机或高压机来制备模塑泡沫或块泡，反应指数是指异氰酸酯基团与相对异氰酸酯基团具有反应活性氢物质的当量数的比值，反应指数是70～80％；Slow resilience foam is formed by fully mixing and reacting MDI system isocyanate and polyether polyol. Low-pressure machine or high-pressure machine is used to prepare molded foam or block foam. The reaction index refers to the reactivity of isocyanate groups and relative isocyanate groups. The ratio of equivalents of hydrogen species, the reaction index is 70-80%; 将聚醚多元醇、发泡剂、表面活性剂、催化剂加入到塑料烧杯中，搅拌均匀后，取一部分于试管中静置、观察稳定情况；保持烧杯中的物料温度24～28℃，然后再加入改性MDI24～28℃，搅拌5～8秒后，迅速倒入铝质模具中，保持模温48-52℃，6～7分脱模，模塑样品的密度约75kg/m3；Add polyether polyol, foaming agent, surfactant, and catalyst into a plastic beaker, stir evenly, take a part of it to stand in a test tube, and observe the stability; keep the temperature of the material in the beaker at 24-28°C, and then Add modified MDI at 24-28°C, stir for 5-8 seconds, then quickly pour it into an aluminum mold, keep the mold temperature at 48-52°C, demould after 6-7 minutes, and the density of the molded sample is about 75kg/m 3 ; 料温控制在24～28℃，MDI体系异氰酸酯流量80～100g/s，聚醚多元醇流量160～180g/s；模具恒温循环水加热，模具温度48-52℃，混合物料注入模具后，6～7min脱模。The material temperature is controlled at 24-28°C, the flow rate of isocyanate in the MDI system is 80-100g/s, and the flow rate of polyether polyol is 160-180g/s; the mold is heated by constant temperature circulating water, and the mold temperature is 48-52°C. ~7min demoulding.
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