A kind of preparation method and products therefrom of closed pore agent
Technical field
The invention belongs to field of porous materials, and in particular to a kind of closed pore agent prepared used in foamed resin.
Background technology
The melamine sponge that market occurred in recent years is also known as melamine sponge, is entered by alkaline melamine resin
The flexible thermosetting foamed plastics of nanoscale three-dimensional cross-linked network made of the foaming of special process microwave.Melamine sponge belongs to
Complete open-celled foam, its percent opening are up to 99.9% fire resistance height, and smoke density is low, be preferable insulation, heat-insulated, sound insulation,
Light material.In the fields such as building decoration, vehicular traffic, water craft, Aero-Space, electromechanical equipment, industrial acoustical absorption heat preserving
Widely used (Wang Dongwei etc., the preparation modification of melamine foams and performance study, functional material, 24 phases in 2012).
Melamine sponge is a new industry in China, and its market demand is huge.According to opening-type on sponge, it is divided into
(eyelet and eyelet be not completely separated by hole wall between each other, has certain for closed pore (not connected between eyelet and eyelet), perforate
Degree together with property) and three kinds of mix aperture (having two kinds of structures of perforate and closed pore concurrently).The open-celled structure water suction of melamine sponge foam
Rate is high to reach 350%, and the foam wt increase after water suction, heat preserving heat insulating noise insulation performance drastically declines, it is easier in cavity
Middle breed bacteria, which produces, goes mouldy, open-celled structure air produce convective heat transfer heat-insulating property it is limited applied in terms of insulation by
Limitation.
Also not specifically for the closed pore agent of melamine sponge on Vehicles Collected from Market.
The content of the invention
For weak point existing for this area, the purpose of the present invention is to propose to a kind of preparation method of closed pore agent.
It is another object of the present invention to propose closed pore agent made from the preparation method.
Third object of the present invention is to propose the application of the closed pore agent
To realize that the technical scheme of above-mentioned purpose of the present invention is:
A kind of preparation method of closed pore agent, including step:
1) to Toluene-2,4-diisocyanate, phthalic anhydride is added in 4- diisocyanate, stirring reaction under normal temperature;The diisocyanate of toluene 2,4 and
The volume mass ratio of phthalic anhydride is 100mL:4~8g;
2) polyethylene glycol 200 is added into reaction system, reaction temperature is 65~75 DEG C, and polyethylene glycol keeps temperature after adding
65~75 DEG C of degree continues reaction and obtains closed pore agent in 30~40 minutes.
Wherein, the toluene di-isocyanate(TDI) is Toluene-2,4-diisocyanate, 4- diisocyanate and/or Toluene-2,4-diisocyanate, 6- diisocyanate.
Generally toluene di-isocyanate(TDI) purchased in market is Toluene-2,4-diisocyanate, 4- diisocyanate and Toluene-2,4-diisocyanate, the mixing of 6- diisocyanate
Thing.But inventor in experiments it is found that, the Toluene-2,4-diisocyanate of high content, 6- diisocyanate add after react dramatic strong, can not control
Reaction process processed, with best containing 80% Toluene-2,4-diisocyanate, 4- diisocyanate effects.
Wherein, the step 1) is additionally added toughener A-60 (Shenzhen gold complete works of Science and Technology Ltd. production), toughener and
Toluene-2,4-diisocyanate, the volume ratio of 4- diisocyanate is 10~20:100.
Wherein, in the step 2), polyethylene glycol and Toluene-2,4-diisocyanate, the volume ratio of 4- diisocyanate is 40~60:100.
Wherein, in the step 2), with the speed control reaction temperature of dropwise addition polyethylene glycol at 68~72 DEG C.
The closed pore agent that preparation method of the present invention is prepared.
Application of the closed pore agent in melamine foams are prepared.
The method for preparing melamine foams using the closed pore agent, including step:According to mass parts, taking can hair style melamine resin
100 parts of (city is available), add 30~40 parts of closed pore agent, 4~6 parts of closed pore adjuvant, 1~3 part of surfactant, curing agent 2
~3 parts, 1~2 part of foaming agent is uniform through high-speed stirred, is placed in microwave in mould and foams.
Wherein, the curing agent is in oxalic acid, formic acid, phosphoric acid, p-methyl benzenesulfonic acid, catalyst for trimerization, ammonium chloride, magnesium sulfate
One or more, the surfactant be dodecyl sodium sulfate, silicone oil, stearic acid, amino acid, poly- sorbic alcohol, fat
One or more in acid glyceride, the foaming agent is pentane, butane, ethane, heptane, dichloroethanes, Arcton 11, two
One or more in dichlorodifluoromethane.
Preferably, the closed pore adjuvant is silicone emulsion, benzoic anhydride polyester polyol, isocyanate than 1:1:0.3
Mixture.
The beneficial effects of the present invention are:
The present invention be directed to existing melamine sponge foam perforate or part open, the problem of causing material fragility big, proposes newly
The preparation method of the closed pore agent of type.
Phthalic anhydride and auxiliary agent are added when preparing closed pore agent, solves the problem of open of melamine foams with the polyurethane of activity.It is made
Closed pore agent can not only effectively reduce melamine sponge percent opening, and improve the toughness of sponge, improve product quality, application
Expand.
Embodiment
Following examples are used to illustrate the present invention, but should not be taken to limit the scope of the present invention.
The equipment component used in embodiment is:Three mouthfuls of reactors, purchased from Jining Heng Tai Chemical Co., Ltd.s;Automatic stirring
Temperature controller, purchased from Jining Heng Tai Chemical Co., Ltd.s;Microwave test machine, purchased from Guangzhou Fu Tao microwave equipments Co., Ltd;Perforate
Rate rate of closed hole measuring instrument, purchased from scientific and technological (Beijing) Co., Ltd of Bei Shide instruments.Toluene in used toluene di-isocyanate(TDI)-
2,4- diisocyanate contents are 80%, and Toluene-2,4-diisocyanate, 4- diisocyanate are designated as in embodiment.
In embodiment, unless otherwise instructed, means used are this area conventional technical means.
Embodiment 1:
Toluene-2,4-diisocyanate is added in beaker, 4- diisocyanate 100ml, adds 5 grams of phthalic anhydride, A-60 (the complete works of science and technology of Shenzhen gold
Co., Ltd produces) after 30 minutes, course of reaction is kept stirring for 15ml normal-temperature reactions.
Polyethylene glycol (molecular weight 200) 50ml is added dropwise to, with the speed control temperature of dropwise addition at 70 DEG C or so, is protected after dripping off
Hold temperature 70 C and continue reaction and obtain closed pore agent in 30 minutes.
Embodiment 2
Take can 100 grams of hair style melamine resin (being purchased from Central Plains great Hua companies of Henan derived energy chemical group), add embodiment 1 make
35 grams of closed pore agent, (silicone emulsion, benzoic anhydride polyester polyol, isocyanate are than 1 for closed pore adjuvant:1:0.3 mixture) 5
Gram, 2 grams of surfactant, 2.4 grams of curing agent ammonium chloride, 1.6 grams of foaming agent pentane, high-speed stirred is uniform.It is placed in micro- in mould
Ripple foams.Obtain the closed pore melamine foams of softness.
The surfactant is:Dodecyl sodium sulfate, silicone oil, stearic acid, amino acid, poly- sorbic alcohol ester 20, fat
One or more in acid glyceride.
Water absorption rate test:The foam for taking length, width and height to be 10cm, it is weighed as 12 grams.Being put into topped up with water in beaker does not have foam
Enter in water, immersion is taken out after 48 hours, and 30 DEG C of temperature are dried in the shade 24 hours, are weighed as 12.1 grams, and water absorption rate is calculated and is
0.83%.
Rate of closed hole is tested:Percent opening rate of closed hole measuring instrument test result is 98.1%.
Embodiment 3:
Toluene-2,4-diisocyanate is added in beaker, 4- diisocyanate 100ml, adds 5 grams of phthalic anhydride, A-60 (the complete works of science and technology of Shenzhen gold
Co., Ltd produces) 15ml, normal-temperature reaction, after 40 minutes, it is kept stirring in course of reaction.
Polyethylene glycol (molecular weight 200) 40ml is added dropwise to, with the speed control temperature of dropwise addition at 72 DEG C, temperature is kept after dripping off
72 DEG C of degree continues reaction and obtains closed pore agent in 30 minutes.
Embodiment 4
Take can 100 grams of hair style melamine resin (being purchased from Central Plains great Hua companies of Henan derived energy chemical group), add embodiment 3 make
30 grams of closed pore agent, (silicone emulsion, benzoic anhydride polyester polyol, isocyanate are than 1 for closed pore adjuvant:1:0.3 mixture) 5
Gram, 2 grams of surfactant (dodecyl sodium sulfate), 2.2 grams of curing agent ammonium chloride, 1.5 grams of foaming agent dichloroethanes, high-speed stirring
Mix uniformly.Microwave in mould is placed in foam.Obtain the closed pore melamine foams of softness.
Water absorption rate test:The foam for taking length, width and height to be 10cm, it is weighed as 12.8 grams.Being put into topped up with water in beaker makes foam
Submerge in water, immersion is taken out after 48 hours, and 30 DEG C of temperature are dried in the shade 24 hours, are weighed as 12.95 grams, and water absorption rate is calculated and is
1.1%.
Rate of closed hole is tested:It is 98.0% with percent opening rate of closed hole measuring instrument test result.
Although above the present invention has made detailed description, on the basis of the present invention, some can be made to it and repaiied
Change or improve, this will be apparent to those skilled in the art.Therefore, institute without departing from theon the basis of the spirit of the present invention
The these modifications or improvements done, belong to the scope of protection of present invention.