CN102827392A - Preparation method of water expanded polystyrene - Google Patents
Preparation method of water expanded polystyrene Download PDFInfo
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Abstract
The invention relates to a preparation method of water expanded polystyrene, and concretely relates to a new method for preparing water expanded polystyrene through using water as a physical foaming agent to substitute an organic pentane foaming agent. Pentane adopted as the foaming agent of traditional expandable polystyrene has a low boiling point, and can be easily released to air in the polystyrene foam material processing and use processes, so the environment in which humans live is polluted. The water expanded polystyrene is prepared through adopting a free radical in-situ copolymerization and free radical suspending polymerization combination method with water as the physical foaming agent in the invention. The method disclosed in the invention has the advantages of no pollution, simple experiment process, ideal foaming effect, very good application prospect, and suitableness for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of water polystyrene foamed.More specifically, relate to a kind of water and replace the novel method that organic pentane foaming agent prepares the water polystyrene foamed as pneumatogen.
Background technology
The consumption of the polystyrene foamed of China mainly concentrates on packing and building field; Account for 50% and 45% respectively, other accounts for 5%, and the polystyrene foamed of developed country be consumed in the building trade accounting up to 70%; Therefore, polystyrene foamed has very vast market prospect in China.
China's polystyrene foamed industry in the world market in occupation of more and more important position.Global polystyrene foamed aggregated capacity was 6,910,000 tons in 2008, and China is 3,100,000 tons, and production capacity accounts for 45% of world's aggregated capacity, by 2010 the end of the year China's polystyrene foamed aggregated capacity ultra surprising especially surpassed 4,500,000 tons.Undoubtedly, China has become the maximum production base of world's polystyrene foamed industry.
Traditional polystyrene foamed is to be whipping agent with the pentane; The main drawback that adopts this organic blowing agent is in the processing and use of polymer materials; Lower boiling pentane is very easy to evaporate in the atmosphere, thereby the environment that we mankind are depended on for existence pollutes.Therefore, in recent years, many scholars propose to use water as the imagination that pneumatogen replaces pentane, and have done some explorations.Prepare environment amenable water polystyrene foamed and mainly contain two kinds of approach; The one, through directly water being introduced the structure that oil phase forms water/oil/water type (W/O/W); The 2nd, through in polymerization process, adding water-absorbing material, it is inner that water is introduced granules of polystyrene through the water sorption of water-absorbing material.
People such as L.Nelissen have carried out deep research to the experimental program and the technology of preparation water polystyrene foamed, and they adopt two kinds of methods successfully to prepare the granules of polystyrene of water foaming.A kind of is directly in styrene monomer, to add emulsified water to carry out the body prepolymerization; When turnover ratio reaches 50% left and right sides; This moment, system had certain viscosity, emulsified water be dispersed in vinylbenzene mutually in, add water carry out suspension polymerization water outlet expanded polystyrene particle this moment; Another kind is earlier synthetic a kind of amphipathic PS-SSS polymeric surface active agent; During polymerization; The PS section of tensio-active agent extend into styrene monomer mutually in; The Lewatit section extend into aqueous phase, and the hydrophilic interaction through sulfonic acid group prepares the water polystyrene foamed with water-dispersion to granules of polystyrene inside.
People such as Hugo Berghmans are with starch, and maleic anhydride, vinylbenzene carry out copolymerization, are maleic anhydride and vinylbenzene on the main chain, and starch is grafted on the main chain through two kinds of approach, and the one, through the hydrogen bond action of hydroxyl in the starch and anhydride bond; The 2nd, the esterification through hydroxyl and anhydride bond is grafted on the main chain, more than simultaneously on the main chain carboxyl.Make through these two kinds of approach and to have contained hydroxyl and two kinds of suctions of carboxyl groups on the vinylbenzene main chain, just can be in polymerization process water-dispersion to granules of polystyrene inside.
L. people such as James Lee has successfully prepared the PS-clay nanocomposites of water foaming through a series of researchs.Mark is at aqueous phase uniformly because of its possess hydrophilic property for natural clay, and through the method for reversed-phase emulsion, clay can further be introduced in the middle mutually reversed-phase emulsion that forms water-in-oil (W/O) of styrene monomer.At last, through suspension polymerization, just prepared the granules of polystyrene that is comprising water/clay.
People such as Jintao Yang have prepared a kind of PS-absorbent charcoal composite material of water foaming; At first; Add the reversed-phase emulsion that styrene monomer prepares water-in-oil (W/O) mutually to the gac that has adsorbed water, gone out comprising the granules of polystyrene of gac/water then through suspension polymerization.
The method for preparing the water polystyrene foamed more than summing up; Need improved place below main the existence; The method that directly adds emulsified water is unfavorable for the dispersion of water, and the polymerization process phenomenon of phase separation is more serious, causes the dispersion of whipping agent water in polymeric matrix even inadequately easily.Also there is the problem that is separated in the method for vinylbenzene and nanoclay or gac blend, and reason is that nanoclay all is mutually inorganic with gac, and vinylbenzene is organic phase, and both are separated seriously, also cause the dispersion of water inhomogeneous easily.Summarize saidly, design a kind of water dispersive preparation method in the PS matrix that helps and be very important.
Summary of the invention
Main purpose of the present invention provides a kind of novel method for preparing the water expanded polystyrene particle; Specifically, mainly be the water expanded polystyrene particle for preparing through the method that nano polypropylene acid absorption resin of sodium microballoon combines with vinylbenzene radical in-situ copolymerization and free radical suspensioning polymerization.
Concrete steps are following:
(1) adopt reversed emulsion polymerization to prepare nano polypropylene acid absorption resin of sodium microballoon.Under condition of ice bath, with in the NaOH solution and vinylformic acid, the control degree of neutralization is at 60-75%; Add the water soluble oxidized reduction initiator potassium persulfate of relative vinylformic acid quality 3% then, the cyclohexane give that adds relative vinylformic acid quality 500% is an external phase, adds the emulsifier span-80 of relative hexanaphthene quality 8%; The linking agent N,N methylene bis acrylamide of relative vinylformic acid quality 0.015%, temperature of reaction is 75 ℃; Stir speed (S.S.) 600-800rpm; N2 condition protection polymerization 4-6 hour down through azeotropic removal of water and external phase hexanaphthene, obtains flaxen product and is ROHM water-absorbing resin microballoon then after the vacuum-drying.
(2) method that adopts radical in-situ copolymerization and free radical suspensioning polymerization to combine prepares the water polystyrene foamed.At first, the nano polypropylene of the relative vinylbenzene quality 0.1%-1% that in styrene monomer, obtains in the dissolving (1) acid absorption resin of sodium microballoon places reaction kettle with mixing solutions; Radical in-situ copolymerization stage initiator Lucidol to wherein adding relative vinylbenzene quality 0.3%-1% is provided with 95 ℃ of temperature, stir speed (S.S.) 800rpm; Radical in-situ copolymerization 0.5-2 hour; To the deionized water that wherein drips relative styrene monomer quality 10%, stir after 0.5 hour then, stir speed (S.S.) transfers to 350rpm; Add free radical suspensioning polymerization stage initiator Lucidol amount 0.3%-3%; The massfraction of styrene monomer adds the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carries out free radical suspensioning polymerization as external phase, polymerization 8 hours relatively.After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.
In this invention, added relative styrene monomer quality 0.1%, 0.3% respectively; 0.5%, 0.7%, 1% nano polypropylene acid absorption resin of sodium microballoon prepares the water expanded polystyrene particle; Experimental result shows that along with the increase of nanometer water-absorbing resin content, the water regain of granules of polystyrene is increasing gradually; This explanation absorbs water microballoon in action, yet the productive rate of granules of polystyrene in the effective size of grain scope but presents the trend that reduces gradually, and this mainly is because of the increase along with suction microballoon amount; The water-swelling effect is more and more obvious, and the unstable of the water/oil when causing suspension polymerization/water (W/O/W) system increases, and causes the part grain breakage easily.Comprehensive this two aspects factor is considered foaming effect simultaneously, and we preferentially select nano polypropylene acid absorption resin of sodium microballoon add-on 0.3%.
The present invention has changed the initiator amount in radical in-situ copolymerization stage, is respectively 0.3%, 0.67%, 1% (massfraction of styrene monomer relatively), and according to experimental result, selection should stage initiator amount 0.67%.
The present invention has changed the time of radical in-situ copolymerization, is respectively 0.5h, 1h, and 1.5h, 2h, according to experimental result, selection should the stage polymerization time be 1h.
This method green non-pollution, experimentation is simple, and foaming effect is desirable, and good application prospects is arranged, and is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the preparation process synoptic diagram of water polystyrene foamed.
Fig. 2 is the dispersion effect synoptic diagram of nano polypropylene acid absorption resin of sodium microballoon in styrene monomer.
Fig. 3 is the microcosmic phase structure sem photograph before the water polystyrene foamed foaming of different nano polypropylenes acid absorption resin of sodium microballoon (PAAS) additions, a wherein, and b, c, the addition of d is respectively 0,0.1%, and 0.3%, 1%.
Fig. 4 is the microcosmic phase structure sem photograph after the water polystyrene foamed foaming of different nano polypropylenes acid absorption resin of sodium microballoon (PAAS) additions, a wherein, and b, c, the addition of d is respectively 0,0.1%, and 0.3%, 0.5%.
Fig. 5 is the curve of differential scanning calorimetric analysis first pass of the water polystyrene foamed of different nano polypropylenes acid absorption resin of sodium microballoon (PAAS) additions, and addition is respectively 0,0.1%, 0.3%, 0.5%.
Fig. 6 is the curve that the differential scanning calorimetric analysis of the water polystyrene foamed of different nano polypropylene acid absorption resin of sodium microballoon (PAAS) additions scans for second time, and addition is respectively 0,0.1%, 0.3%, 0.5%.
Fig. 7 is the thermogravimetic analysis (TGA) curve of the water polystyrene foamed of different nano polypropylene acid absorption resin of sodium microballoon (PAAS) additions, and addition is respectively 0,0.1%, 0.3%, 0.5%.
Embodiment
Instance one: adopt reversed emulsion polymerization to prepare nano polypropylene acid absorption resin of sodium microballoon.Under condition of ice bath, with in the NaOH solution and vinylformic acid, the control degree of neutralization is 60%; Add the water soluble oxidized reduction initiator potassium persulfate of relative vinylformic acid quality 3% then, the cyclohexane give that adds relative vinylformic acid quality 500% is an external phase, adds the emulsifier span-80 of relative hexanaphthene quality 8%; The linking agent N,N methylene bis acrylamide of relative vinylformic acid quality 0.015%, temperature of reaction is 75 ℃; Stir speed (S.S.) 800rpm, N
2Polymerization is 5 hours under the condition protection, through azeotropic removal of water and external phase hexanaphthene, obtains flaxen product after the vacuum-drying and is ROHM water-absorbing resin microballoon then.Under the electron microscope, particle diameter is about 60nm.
Instance two: adopt reversed emulsion polymerization to prepare nano polypropylene acid absorption resin of sodium microballoon.Under condition of ice bath, with in the NaOH solution and vinylformic acid, the control degree of neutralization is 75%; Add the water soluble oxidized reduction initiator potassium persulfate of relative vinylformic acid quality 3% then, the cyclohexane give that adds relative vinylformic acid quality 500% is an external phase, adds the emulsifier span-80 of relative hexanaphthene quality 8%; The linking agent N,N methylene bis acrylamide of relative vinylformic acid quality 0.015%, temperature of reaction is 75 ℃; Stir speed (S.S.) 800rpm, N
2Polymerization is 5 hours under the condition protection, through azeotropic removal of water and external phase hexanaphthene, obtains flaxen product after the vacuum-drying and is ROHM water-absorbing resin microballoon then.Under the electron microscope, particle diameter is about 70nm.
Instance three: adopt reversed emulsion polymerization to prepare nano polypropylene acid absorption resin of sodium microballoon.Under condition of ice bath, with in the NaOH solution and vinylformic acid, the control degree of neutralization is 65%; Add the water soluble oxidized reduction initiator potassium persulfate of relative vinylformic acid quality 3% then, the cyclohexane give that adds relative vinylformic acid quality 500% is an external phase, adds the emulsifier span-80 of relative hexanaphthene quality 8%; The linking agent N,N methylene bis acrylamide of relative vinylformic acid quality 0.015%, temperature of reaction is 75 ℃; Stir speed (S.S.) 600rpm, N
2Polymerization is 5 hours under the condition protection, through azeotropic removal of water and external phase hexanaphthene, obtains flaxen product after the vacuum-drying and is ROHM water-absorbing resin microballoon then.Under the electron microscope, particle diameter is about 75nm.
Instance four: adopt reversed emulsion polymerization to prepare nano polypropylene acid absorption resin of sodium microballoon.Under condition of ice bath, with in the NaOH solution and vinylformic acid, the control degree of neutralization is 65%; Add the water soluble oxidized reduction initiator potassium persulfate of relative vinylformic acid quality 3% then, the cyclohexane give that adds relative vinylformic acid quality 500% is an external phase, adds the emulsifier span-80 of relative hexanaphthene quality 8%; The linking agent N,N methylene bis acrylamide of relative vinylformic acid quality 0.015%, temperature of reaction is 75 ℃; Stir speed (S.S.) 800rpm, N
2Polymerization is 4 hours under the condition protection, through azeotropic removal of water and external phase hexanaphthene, obtains flaxen product after the vacuum-drying and is ROHM water-absorbing resin microballoon then.Under the electron microscope, particle diameter is about 40nm.
Instance five: adopt reversed emulsion polymerization to prepare nano polypropylene acid absorption resin of sodium microballoon.Under condition of ice bath, with in the NaOH solution and vinylformic acid, the control degree of neutralization is 65%; Add the water soluble oxidized reduction initiator potassium persulfate of relative vinylformic acid quality 3% then, the cyclohexane give that adds relative vinylformic acid quality 500% is an external phase, adds the emulsifier span-80 of relative hexanaphthene quality 8%; The linking agent N,N methylene bis acrylamide of relative vinylformic acid quality 0.015%, temperature of reaction is 75 ℃; Stir speed (S.S.) 800rpm, N
2Polymerization is 6 hours under the condition protection, through azeotropic removal of water and external phase hexanaphthene, obtains flaxen product after the vacuum-drying and is ROHM water-absorbing resin microballoon then.Under the electron microscope, particle diameter is about 50nm.
Below the absorption resin of sodium polyacrylate microballoon of preparation in our use-case five prepare water base foamed polystyrene resin particle.
Instance six: at first, the nano polypropylene of relative vinylbenzene quality 0.1% acid absorption resin of sodium microballoon is dissolved in the styrene monomer, mixing solutions is placed reaction kettle; To the radical in-situ copolymerization stage initiator Lucidol that wherein adds relative vinylbenzene quality 0.67%; 95 ℃ of temperature are set, stir speed (S.S.) 800rpm, polymerization 1 hour; Then to the deionized water that wherein drips relative vinylbenzene quality 10% as whipping agent; Stir after 0.5 hour, stir speed (S.S.) transfers to 350rpm, adds the free radical suspensioning polymerization stage initiator Lucidol amount of relative vinylbenzene quality 1%; Add the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carry out free radical suspensioning polymerization as external phase, polymerization 8 hours.After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.Obtain water base polystyrene foamed, water-absorbing resin microballoon dispersed fine in matrix, water cut is 3.54%, and second-order transition temperature is 102.1 ℃, and the oil bath expansion ratio is 4.28.
Instance seven: at first, the nano polypropylene of relative vinylbenzene quality 1% acid absorption resin of sodium microballoon is dissolved in the styrene monomer, mixing solutions is placed reaction kettle; To the radical in-situ copolymerization stage initiator Lucidol that wherein adds relative vinylbenzene quality 0.67%; 95 ℃ of temperature are set, stir speed (S.S.) 800rpm, polymerization 1 hour; Then to the deionized water that wherein drips relative vinylbenzene quality 10% as whipping agent; Stir after 0.5 hour, stir speed (S.S.) transfers to 350rpm, adds the free radical suspensioning polymerization stage initiator Lucidol amount of relative vinylbenzene quality 1%; Add the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carry out free radical suspensioning polymerization as external phase, polymerization 8 hours.After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.Obtain water base polystyrene foamed, the dispersiveness of water-absorbing resin microballoon in matrix is general, and water cut is 6.54%, and second-order transition temperature is 104.6 ℃, and the oil bath expansion ratio is 3.29.
Instance eight: at first, the nano polypropylene of relative vinylbenzene quality 0.3% acid absorption resin of sodium microballoon is dissolved in the styrene monomer, mixing solutions is placed reaction kettle; To the radical in-situ copolymerization stage initiator Lucidol that wherein adds relative vinylbenzene quality 0.3%; 95 ℃ of temperature are set, stir speed (S.S.) 800rpm, polymerization 1 hour; Then to the deionized water that wherein drips relative vinylbenzene quality 10% as whipping agent; Stir after 0.5 hour, stir speed (S.S.) transfers to 350rpm, adds the free radical suspensioning polymerization stage initiator Lucidol amount of relative vinylbenzene quality 1%; Add the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carry out free radical suspensioning polymerization as external phase, polymerization 8 hours.After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.Obtain water base polystyrene foamed, the good dispersivity of water-absorbing resin microballoon in matrix, water cut is 4.94%, and second-order transition temperature is 103.2 ℃, and the oil bath expansion ratio is 6.37.
Instance nine: at first, the nano polypropylene of relative vinylbenzene quality 0.5% acid absorption resin of sodium microballoon is dissolved in the styrene monomer, mixing solutions is placed reaction kettle; To the radical in-situ copolymerization stage initiator Lucidol that wherein adds relative vinylbenzene quality 1%; 95 ℃ of temperature are set, stir speed (S.S.) 800rpm, polymerization 1 hour; Then to the deionized water that wherein drips relative vinylbenzene quality 10% as whipping agent; Stir after 0.5 hour, stir speed (S.S.) transfers to 350rpm, adds the free radical suspensioning polymerization stage initiator Lucidol amount of relative vinylbenzene quality 1%; Add the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carry out free radical suspensioning polymerization as external phase, polymerization 8 hours.After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.Obtain water base polystyrene foamed, the dispersiveness of water-absorbing resin microballoon in matrix is general, and water cut is 6.03%, and second-order transition temperature is 104.2 ℃, and the oil bath expansion ratio is 4.08.
Instance ten: at first, the nano polypropylene of relative vinylbenzene quality 0.3% acid absorption resin of sodium microballoon is dissolved in the styrene monomer, mixing solutions is placed reaction kettle; To the radical in-situ copolymerization stage initiator Lucidol that wherein adds relative vinylbenzene quality 0.3%; 95 ℃ of temperature are set, stir speed (S.S.) 800rpm, polymerization 2 hours; Then to the deionized water that wherein drips relative vinylbenzene quality 10% as whipping agent; Stir after 0.5 hour, stir speed (S.S.) transfers to 350rpm, adds the free radical suspensioning polymerization stage initiator Lucidol amount of relative vinylbenzene quality 1%; Add the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carry out free radical suspensioning polymerization as external phase, polymerization 8 hours.After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.Obtain water base polystyrene foamed, the good dispersivity of water-absorbing resin microballoon in matrix, water cut is 4.53%, and second-order transition temperature is 103.5 ℃, and the oil bath expansion ratio is 5.73.
Instance 11: at first, the nano polypropylene of relative vinylbenzene quality 0.3% acid absorption resin of sodium microballoon is dissolved in the styrene monomer, mixing solutions is placed reaction kettle; To the radical in-situ copolymerization stage initiator Lucidol that wherein adds relative vinylbenzene quality 0.67%; 95 ℃ of temperature are set, stir speed (S.S.) 800rpm, polymerase 10 .5 hour; Then to the deionized water that wherein drips relative vinylbenzene quality 10% as whipping agent; Stir after 0.5 hour, stir speed (S.S.) transfers to 350rpm, adds the free radical suspensioning polymerization stage initiator Lucidol amount of relative vinylbenzene quality 2%; Add the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carry out free radical suspensioning polymerization as external phase, polymerization 8 hours.After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.Obtain water base polystyrene foamed, the good dispersivity of water-absorbing resin microballoon in matrix, water cut is 4.23%, and second-order transition temperature is 103.7 ℃, and the oil bath expansion ratio is 4.32.
Below the absorption resin of sodium polyacrylate microballoon of preparation in our use-case four prepare water base foamed polystyrene resin particle.
Instance 12: at first, the nano polypropylene of relative vinylbenzene quality 0.1% acid absorption resin of sodium microballoon is dissolved in the styrene monomer, mixing solutions is placed reaction kettle; To the radical in-situ copolymerization stage initiator Lucidol that wherein adds relative vinylbenzene quality 0.67%; 95 ℃ of temperature are set, stir speed (S.S.) 800rpm, polymerization 2 hours; Then to the deionized water that wherein drips relative vinylbenzene quality 10% as whipping agent; Stir after 0.5 hour, stir speed (S.S.) transfers to 350rpm, adds the free radical suspensioning polymerization stage initiator Lucidol amount of relative vinylbenzene quality 1%; Add the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carry out free radical suspensioning polymerization as external phase, polymerization 8 hours.After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.Obtain water base polystyrene foamed, the good dispersivity of water-absorbing resin microballoon in matrix, water cut is 3.15%, and second-order transition temperature is 102.4 ℃, and the oil bath expansion ratio is 3.98.
Below the absorption resin of sodium polyacrylate microballoon of preparation in our use-case three prepare water base foamed polystyrene resin particle.
Instance 13: at first, the nano polypropylene of relative vinylbenzene quality 0.5% acid absorption resin of sodium microballoon is dissolved in the styrene monomer, mixing solutions is placed reaction kettle; To the radical in-situ copolymerization stage initiator Lucidol that wherein adds relative vinylbenzene quality 0.67%; 95 ℃ of temperature are set, stir speed (S.S.) 800rpm, polymerization 1 hour; Then to the deionized water that wherein drips relative vinylbenzene quality 10% as whipping agent; Stir after 0.5 hour, stir speed (S.S.) transfers to 350rpm, adds the free radical suspensioning polymerization stage initiator Lucidol amount of relative vinylbenzene quality 0.3%; Add the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carry out free radical suspensioning polymerization as external phase, polymerization 8 hours.After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.Obtain water base polystyrene foamed, the dispersiveness of water-absorbing resin microballoon in matrix is general, and water cut is 6.13%, and second-order transition temperature is 104.8 ℃, and the oil bath expansion ratio is 4.07.
Below the absorption resin of sodium polyacrylate microballoon of preparation in our use-case two prepare water base foamed polystyrene resin particle.
Instance 14: at first, the nano polypropylene of relative vinylbenzene quality 0.3% acid absorption resin of sodium microballoon is dissolved in the styrene monomer, mixing solutions is placed reaction kettle; To the radical in-situ copolymerization stage initiator Lucidol that wherein adds relative vinylbenzene quality 0.67%; 95 ℃ of temperature are set, stir speed (S.S.) 800rpm, polymerization 1 hour; Then to the deionized water that wherein drips relative vinylbenzene quality 10% as whipping agent; Stir after 0.5 hour, stir speed (S.S.) transfers to 350rpm, adds the free radical suspensioning polymerization stage initiator Lucidol amount of relative vinylbenzene quality 1%; Add the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carry out free radical suspensioning polymerization as external phase, polymerization 8 hours.After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.Obtain water base polystyrene foamed, the good dispersivity of water-absorbing resin microballoon in matrix, water cut is 5.04%, and second-order transition temperature is 103.6 ℃, and the oil bath expansion ratio is 5.63.
Below the absorption resin of sodium polyacrylate microballoon of preparation in our use-case one prepare water base foamed polystyrene resin particle.
Instance 15: at first, the nano polypropylene of relative vinylbenzene quality 0.1% acid absorption resin of sodium microballoon is dissolved in the styrene monomer, mixing solutions is placed reaction kettle; To the radical in-situ copolymerization stage initiator Lucidol that wherein adds relative vinylbenzene quality 0.67%; 95 ℃ of temperature are set, stir speed (S.S.) 800rpm, polymerization 1 hour; Then to the deionized water that wherein drips relative vinylbenzene quality 10% as whipping agent; Stir after 0.5 hour, stir speed (S.S.) transfers to 350rpm, adds the free radical suspensioning polymerization stage initiator Lucidol amount of relative vinylbenzene quality 3%; Add the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carry out free radical suspensioning polymerization as external phase, polymerization 8 hours.After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.Obtain water base polystyrene foamed, the good dispersivity of water-absorbing resin microballoon in matrix, water cut is 3.2%, and second-order transition temperature is 102.7 ℃, and the oil bath expansion ratio is 3.36.
Claims (5)
1. the preparation method of a water polystyrene foamed is characterized in that step is following:
(1) adopt reversed emulsion polymerization to prepare nano polypropylene acid absorption resin of sodium microballoon: under condition of ice bath,, to control degree of neutralization at 60-75% with in the NaOH solution and vinylformic acid; The water soluble oxidized reduction initiator potassium persulfate that adds relative vinylformic acid quality 3% then; The cyclohexane give that adds relative vinylformic acid quality 500% is an external phase, adds the emulsifier span-80 of relative hexanaphthene quality 8%, relatively the linking agent N of vinylformic acid quality 0.015%; The N-methylene-bisacrylamide; Temperature of reaction is 75 ℃, stir speed (S.S.) 600-800rpm, N
2Condition protection polymerization 4-6 hour down through azeotropic removal of water and external phase hexanaphthene, obtains flaxen product and is the absorption resin of sodium polyacrylate microballoon then after the vacuum-drying;
(2) method that adopts radical in-situ copolymerization and free radical suspensioning polymerization to combine prepares the water polystyrene foamed: at first; The nano polypropylene acid absorption resin of sodium microballoon of the relative vinylbenzene quality 0.1%-1% that obtains in the dissolving step in styrene monomer (1); To the radical in-situ copolymerization stage initiator Lucidol that wherein adds relative vinylbenzene quality 0.3%-1%; 95 ℃ of temperature are set, stir speed (S.S.) 800rpm, radical in-situ copolymerization 0.5-2 hour; Then to the deionized water that wherein drips relative styrene monomer quality 10%; Stir after 0.5 hour, stir speed (S.S.) transfers to 350rpm, adds the free radical suspensioning polymerization stage initiator Lucidol of relative vinylbenzene quality 0.3%-3%; Add the mixed aqueous solution that is dissolved with 0.12% suspension stabilizer Natvosol and 0.3% tricalcium phosphate and carry out free radical suspensioning polymerization as external phase, polymerization 8 hours; After the finishing polymerization, the filtration washing product promptly gets the water polystyrene foamed.
2. the preparation method of a kind of water polystyrene foamed according to claim 1 is characterized in that adding the nano polypropylene acid absorption resin of sodium microballoon of relative styrene monomer quality 0.3%.
3. the preparation method of a kind of water polystyrene foamed according to claim 1 is characterized in that adding the radical in-situ copolymerization stage initiator Lucidol of relative styrene monomer quality 0.67%.
4. the preparation method of a kind of water polystyrene foamed according to claim 1 is characterized in that the radical in-situ copolymerization time is 1h.
5. the preparation method of a kind of water polystyrene foamed according to claim 1 is characterized in that adding the free radical suspensioning polymerization stage initiator Lucidol of relative styrene monomer quality 1%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104927275A (en) * | 2015-05-26 | 2015-09-23 | 湖州佳宁印刷有限公司 | Water-based foaming polystyrene material with starch as water carrier and preparation method of water-based foaming polystyrene material |
| CN111995789A (en) * | 2020-03-25 | 2020-11-27 | 武汉纺织大学 | Hydrophilic resin for catalytic degradation of antibiotics and preparation method and application thereof |
| CN113430713A (en) * | 2021-05-21 | 2021-09-24 | 徐恩淼 | Composite board with electromagnetic shielding performance and preparation method thereof |
-
2012
- 2012-05-18 CN CN 201210157693 patent/CN102827392B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 金峰等: "苯乙烯/聚丙烯酸钠原位聚合物的水崩解性研究", 《塑料工业》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104927275A (en) * | 2015-05-26 | 2015-09-23 | 湖州佳宁印刷有限公司 | Water-based foaming polystyrene material with starch as water carrier and preparation method of water-based foaming polystyrene material |
| CN111995789A (en) * | 2020-03-25 | 2020-11-27 | 武汉纺织大学 | Hydrophilic resin for catalytic degradation of antibiotics and preparation method and application thereof |
| CN111995789B (en) * | 2020-03-25 | 2022-09-27 | 武汉纺织大学 | Hydrophilic resin for catalytic degradation of antibiotics and preparation method and application thereof |
| CN113430713A (en) * | 2021-05-21 | 2021-09-24 | 徐恩淼 | Composite board with electromagnetic shielding performance and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102827392B (en) | 2013-10-30 |
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