CN100497430C - Method of preparing full MDI polyurethane slow rebound foam - Google Patents
Method of preparing full MDI polyurethane slow rebound foam Download PDFInfo
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Abstract
The invention discloses a making method of full-MDI polyurethane slow-rebound foam in the polyurethane foam making technical domain, which comprises the following parts: a. MDI system isocyanate with functional degree at 2.1-2.5, b. polyether polyol, c. foamer, d, catalyst and surface activator, wherein the composite polyether consists of bulk polyether product and relative adjuvant without physical foamer, which can be reserved as pillow, bustle and mattress for a long time.
Description
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
*" 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
Claims (6)
1, the preparation method of all-MDI polyurethane low resilience urethane foam resilient foam, raw material is formed and is comprised following component:
A.MDI system isocyanate, functionality are 2.1～2.5;
B. polyether glycol;
C. whipping agent;
D. catalyzer and tensio-active agent;
Be characterised in that 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 are greater than 50%, and functionality is 3, hydroxyl value 35～56mg KOH/g;
The polyol of polyol E propylene oxide, oxyethane, EO content are greater than 50%, and functionality is 3, hydroxyl value 112～240mg KOH/g;
The part by weight of the relative polyether glycol total amount of various polyvalent alcohols is that the weight content of polyol A 30～50%, polyol B5～10%, polyol C40～60%, polyol D+polyol E is 5～10%, and the ratio of polyolD/polyol E weight content is 0.14～0.35.
2,, be characterised in that whipping agent is H according to the preparation method of the described all-MDI polyurethane low resilience urethane foam resilient foam of claim 1
2In O, pentane, the methylene dichloride one or more, consumption are the weight ratio 1～3% with respect to 100 parts of polyether glycols.
3, according to the preparation method of the described all-MDI polyurethane low resilience urethane foam resilient foam of claim 1, be characterised in that described tensio-active agent is the common soft bubble of preparation urethane and the tensio-active agent of high resilience, consumption is the weight ratio 0.5～1.0% of relative polyether glycol total amount.
4, according to the preparation method of the described all-MDI polyurethane low resilience urethane foam resilient foam of claim 1, be characterised in that catalyzer is two (dimethylamino ethyl) ethers, five methyl diethylentriamine, N, N '-dimethylcyclohexylamine, triethylene diamine, stannous octoate, dibutyl tin laurate, selecting wherein, one or more mix use.
5, according to the preparation method of the described all-MDI polyurethane low resilience urethane foam resilient foam of claim 1, be characterised in that in the preparation of low resilience urethane foam resilient foam and also use chainextender and linking agent, chainextender is the small molecules polyvalent alcohol or the aminated compounds of two functionality, and consumption 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, and consumption is the weight ratio 0.5～1.5% of relative polyether glycol total amount.
6, according to the preparation method of the described all-MDI polyurethane low resilience urethane foam resilient foam of claim 1, be characterised in that
Low resilience urethane foam resilient foam is to form through MDI system isocyanate and the reaction of polyether glycol thorough mixing, adopt low press or high-pressure unit to prepare moulded foam or piece bubble, index of Response is meant that isocyanate groups and relative isocyanate groups have the ratio of the equivalents of reactive hydrogens material, and index of Response is 70～80%;
Polyether glycol, 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 ℃, MDI system isocyanate flow 80～100g/s, polyether glycol flow 160～180g/s; The heating of mould thermostatical circulating water, die temperature 48-52 ℃, after mixture injects mould, 6～7min demoulding.
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2006
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