CN102827392B - Preparation method of water expanded polystyrene - Google Patents
Preparation method of water expanded polystyrene Download PDFInfo
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- CN102827392B CN102827392B CN 201210157693 CN201210157693A CN102827392B CN 102827392 B CN102827392 B CN 102827392B CN 201210157693 CN201210157693 CN 201210157693 CN 201210157693 A CN201210157693 A CN 201210157693A CN 102827392 B CN102827392 B CN 102827392B
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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 steeping in water for reconstitution foamed polystyrene.More specifically, relate to a kind of water and replace the novel method that organic pentane foaming agent prepares the steeping in water for reconstitution foamed polystyrene as pneumatogen.
Background technology
The consumption of the polystyrene foamed of China mainly concentrates on packing and building field, account for respectively 50% and 45%, 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 wide market outlook in China.
China's polystyrene foamed industry in the world market in occupation of consequence more and more.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 super surprisingly especially surpassed 4,500,000 tons.Undoubtedly, China has become the production base of world's polystyrene foamed industry maximum.
Traditional polystyrene foamed is as whipping agent take pentane, the main drawback that adopts this organic blowing agent is in the processing and use procedure of polymer materials, lower boiling pentane is very easy to evaporate in the atmosphere, thus the environment that we mankind are depended on for existence.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 steeping in water for reconstitution foamed polystyrene and mainly contain two kinds of approach, the one, by directly water being introduced the structure of oil phase formation water/oil/water type (W/O/W), the 2nd, by add water-absorbing material in polymerization process, it is inner that water is introduced granules of polystyrene by the water sorption of water-absorbing material.
The people such as L.Nelissen conduct in-depth research experimental program and the technique of preparation steeping in water for reconstitution foamed polystyrene, and they adopt two kinds of methods successfully to prepare the granules of polystyrene of steeping in water for reconstitution bubble.A kind of is directly to add emulsified water to carry out bulk prepolymerization in styrene monomer, 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 this moment and carry out suspension polymerization and prepare steeping in water for reconstitution foamed polystyrene particle; Another kind is to synthesize first a kind of amphipathic Polystyrene-styrene sodium sulfonate polymeric surface active agent, during polymerization, the polystyrene section of tensio-active agent extend into styrene monomer mutually in, the sodium polystyrene sulfonate section extend into aqueous phase, and the hydrophilic interaction by sulfonic acid group prepares the steeping in water for reconstitution foamed polystyrene with water-dispersion to granules of polystyrene inside.
The 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 by two kinds of approach, and the one, by the hydrogen bond action of hydroxyl in the starch and anhydride bond; The 2nd, the esterification by hydroxyl and anhydride bond is grafted on the main chain, more than simultaneously on the main chain carboxyl.By these two kinds of approach so that contained hydroxyl on the vinylbenzene main chain and two kinds of carboxyls suction groups, just can be water-dispersion to granules of polystyrene inside in polymerization process.
L. the people such as James Lee has successfully prepared the polystyrene-clay nanocomposites of steeping in water for reconstitution bubble by a series of researchs.Mark is at aqueous phase uniformly because it has wetting ability for natural clay, and by the method for reversed-phase emulsion, clay can further be introduced in the mutually middle reversed-phase emulsion that forms water-in-oil (W/O) of styrene monomer.At last, by suspension polymerization, just prepared the granules of polystyrene that is comprising water/clay.
The people such as Jintao Yang have prepared a kind of polystyrene-absorbent charcoal composite material of steeping in water for reconstitution bubble, at first, the gac that has adsorbed water is added the reversed-phase emulsion that styrene monomer prepares water-in-oil (W/O) mutually, then prepared the granules of polystyrene that is comprising gac/water by suspension polymerization.
The method for preparing the steeping in water for reconstitution foamed polystyrene 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 easily the dispersion of whipping agent water in polymeric matrix even not.Also there is the problem that is separated in the method for vinylbenzene and nanoclay or gac blend, and reason is that nanoclay and gac all are inorganic phases, and vinylbenzene is organic phase, and both are separated seriously, also cause easily the dispersion of water inhomogeneous.Summarize describedly, design and a kind ofly be conducive to the preparation method that water disperses be very important in the polystyrene matrix.
Summary of the invention
Main purpose of the present invention provides a kind of novel method for preparing steeping in water for reconstitution foamed polystyrene particle, specifically, mainly be the steeping in water for reconstitution foamed polystyrene particle for preparing by the method that nano polypropylene acid absorption resin of sodium microballoon combines with vinylbenzene free radical in-situ copolymerization and free radical suspensioning polymerization.
Concrete steps are as follows:
(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%; then the water soluble oxidized reduction initiator potassium persulfate that adds relative vinylformic acid quality 3%; the cyclohexane give that adds relative vinylformic acid quality 500% is external phase; the emulsifier span-80 that adds relative hexanaphthene quality 8%; the linking agent N of relative vinylformic acid quality 0.015%; the N-methylene-bisacrylamide; temperature of reaction is 75 ℃, stir speed (S.S.) 600-800rpm, lower polymerization 4-6 hour of N2 condition protection; then by azeotropic removal of water and external phase hexanaphthene, obtain flaxen product after the vacuum-drying and be polyacrylic acid water-absorbing resin microballoon.
(2) method that adopts free radical in-situ copolymerization and free radical suspensioning polymerization to combine prepares the steeping in water for reconstitution foamed polystyrene.At first, the nano polypropylene acid absorption resin of sodium microballoon of the relative vinylbenzene quality 0.1%-1% that in styrene monomer, obtains in the dissolving (1), mixing solutions is placed reactor, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 0.3%-1%, 95 ℃ of set temperatures, stir speed (S.S.) 800rpm, free 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, add free radical suspensioning polymerization stage initiator benzoyl peroxide 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.
In this invention, added respectively relative styrene monomer quality 0.1%, 0.3%, 0.5%, 0.7%, 1% nano polypropylene acid absorption resin of sodium microballoon prepares steeping in water for reconstitution foamed 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 suction 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 that the water-swelling effect is more and more obvious because of the increase along with suction microballoon amount, the unstable of the water/oil when causing suspension polymerization/water (W/O/W) system increases, and causes easily the part grain breakage.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 free radical in-situ copolymerization stage, is respectively the massfraction of the relative styrene monomer of 0.3%, 0.67%, 1%(), according to experimental result, select this stage initiator amount 0.67%.
The present invention has changed the time of free radical in-situ copolymerization, is respectively 0.5h, 1h, and 1.5h, 2h, according to experimental result, selecting this stage polymerization time is 1h.
The method green non-pollution, experimentation is simple, and foaming effect is desirable, and good application prospect is arranged, and is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the preparation process synoptic diagram of steeping in water for reconstitution foamed polystyrene.
Fig. 2 is the dispersion effect synoptic diagram of nano polypropylene acid absorption resin of sodium microballoon in styrene monomer.
Fig. 3 is the micro structure scanning electron microscope (SEM) photograph before the steeping in water for reconstitution foamed polystyrene 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 micro structure scanning electron microscope (SEM) photograph after the steeping in water for reconstitution foamed polystyrene 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 steeping in water for reconstitution foamed polystyrene 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 steeping in water for reconstitution foamed polystyrene 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 steeping in water for reconstitution foamed polystyrene of different nano polypropylene acid absorption resin of sodium microballoon (PAAS) additions, and addition is respectively 0,0.1%, 0.3%, 0.5%.
Embodiment
Example 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, then the control degree of neutralization adds the water soluble oxidized reduction initiator potassium persulfate of relative vinylformic acid quality 3% 60%, and the cyclohexane give that adds relative vinylformic acid quality 500% is external phase, the emulsifier span-80 that adds 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
2The lower polymerization of condition protection 5 hours then by azeotropic removal of water and external phase hexanaphthene, obtains flaxen product and is polyacrylic acid water-absorbing resin microballoon after the vacuum-drying.Under the electron microscope, particle diameter is about 60nm.
Example 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, then the control degree of neutralization adds the water soluble oxidized reduction initiator potassium persulfate of relative vinylformic acid quality 3% 75%, and the cyclohexane give that adds relative vinylformic acid quality 500% is external phase, the emulsifier span-80 that adds 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
2The lower polymerization of condition protection 5 hours then by azeotropic removal of water and external phase hexanaphthene, obtains flaxen product and is polyacrylic acid water-absorbing resin microballoon after the vacuum-drying.Under the electron microscope, particle diameter is about 70nm.
Example 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, then the control degree of neutralization adds the water soluble oxidized reduction initiator potassium persulfate of relative vinylformic acid quality 3% 65%, and the cyclohexane give that adds relative vinylformic acid quality 500% is external phase, the emulsifier span-80 that adds 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
2The lower polymerization of condition protection 5 hours then by azeotropic removal of water and external phase hexanaphthene, obtains flaxen product and is polyacrylic acid water-absorbing resin microballoon after the vacuum-drying.Under the electron microscope, particle diameter is about 75nm.
Example 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, then the control degree of neutralization adds the water soluble oxidized reduction initiator potassium persulfate of relative vinylformic acid quality 3% 65%, and the cyclohexane give that adds relative vinylformic acid quality 500% is external phase, the emulsifier span-80 that adds 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
2The lower polymerization of condition protection 4 hours then by azeotropic removal of water and external phase hexanaphthene, obtains flaxen product and is polyacrylic acid water-absorbing resin microballoon after the vacuum-drying.Under the electron microscope, particle diameter is about 40nm.
Example 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, then the control degree of neutralization adds the water soluble oxidized reduction initiator potassium persulfate of relative vinylformic acid quality 3% 65%, and the cyclohexane give that adds relative vinylformic acid quality 500% is external phase, the emulsifier span-80 that adds 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
2The lower polymerization of condition protection 6 hours then by azeotropic removal of water and external phase hexanaphthene, obtains flaxen product and is polyacrylic acid water-absorbing resin microballoon after the vacuum-drying.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.
Example six: at first, the nano polypropylene acid absorption resin of sodium microballoon of relative vinylbenzene quality 0.1% is dissolved in the styrene monomer, mixing solutions is placed reactor, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 0.67%, 95 ℃ of set temperatures, 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, the free radical suspensioning polymerization stage initiator benzoyl peroxide amount that adds 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.Obtain water base polystyrene foamed, dispersed fine in matrix of water-absorbing resin microballoon, water content is 3.54%, and second-order transition temperature is 102.1 ℃, and the oil bath expansion ratio is 4.28.
Example seven: at first, the nano polypropylene acid absorption resin of sodium microballoon of relative vinylbenzene quality 1% is dissolved in the styrene monomer, mixing solutions is placed reactor, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 0.67%, 95 ℃ of set temperatures, 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, the free radical suspensioning polymerization stage initiator benzoyl peroxide amount that adds 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.Obtain water base polystyrene foamed, the dispersiveness of water-absorbing resin microballoon in matrix is general, and water content is 6.54%, and second-order transition temperature is 104.6 ℃, and the oil bath expansion ratio is 3.29.
Example eight: at first, the nano polypropylene acid absorption resin of sodium microballoon of relative vinylbenzene quality 0.3% is dissolved in the styrene monomer, mixing solutions is placed reactor, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 0.3%, 95 ℃ of set temperatures, 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, the free radical suspensioning polymerization stage initiator benzoyl peroxide amount that adds 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.Obtain water base polystyrene foamed, the good dispersity of water-absorbing resin microballoon in matrix, water content is 4.94%, and second-order transition temperature is 103.2 ℃, and the oil bath expansion ratio is 6.37.
Example nine: at first, the nano polypropylene acid absorption resin of sodium microballoon of relative vinylbenzene quality 0.5% is dissolved in the styrene monomer, mixing solutions is placed reactor, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 1%, 95 ℃ of set temperatures, 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, the free radical suspensioning polymerization stage initiator benzoyl peroxide amount that adds 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.Obtain water base polystyrene foamed, the dispersiveness of water-absorbing resin microballoon in matrix is general, and water content is 6.03%, and second-order transition temperature is 104.2 ℃, and the oil bath expansion ratio is 4.08.
Example ten: at first, the nano polypropylene acid absorption resin of sodium microballoon of relative vinylbenzene quality 0.3% is dissolved in the styrene monomer, mixing solutions is placed reactor, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 0.3%, 95 ℃ of set temperatures, 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, the free radical suspensioning polymerization stage initiator benzoyl peroxide amount that adds 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.Obtain water base polystyrene foamed, the good dispersity of water-absorbing resin microballoon in matrix, water content is 4.53%, and second-order transition temperature is 103.5 ℃, and the oil bath expansion ratio is 5.73.
Example 11: at first, the nano polypropylene acid absorption resin of sodium microballoon of relative vinylbenzene quality 0.3% is dissolved in the styrene monomer, mixing solutions is placed reactor, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 0.67%, 95 ℃ of set temperatures, 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, the free radical suspensioning polymerization stage initiator benzoyl peroxide amount that adds 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.Obtain water base polystyrene foamed, the good dispersity of water-absorbing resin microballoon in matrix, water content 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.
Example 12: at first, the nano polypropylene acid absorption resin of sodium microballoon of relative vinylbenzene quality 0.1% is dissolved in the styrene monomer, mixing solutions is placed reactor, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 0.67%, 95 ℃ of set temperatures, 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, the free radical suspensioning polymerization stage initiator benzoyl peroxide amount that adds 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.Obtain water base polystyrene foamed, the good dispersity of water-absorbing resin microballoon in matrix, water content 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.
Example 13: at first, the nano polypropylene acid absorption resin of sodium microballoon of relative vinylbenzene quality 0.5% is dissolved in the styrene monomer, mixing solutions is placed reactor, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 0.67%, 95 ℃ of set temperatures, 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, the free radical suspensioning polymerization stage initiator benzoyl peroxide amount that adds 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.Obtain water base polystyrene foamed, the dispersiveness of water-absorbing resin microballoon in matrix is general, and water content 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.
Example 14: at first, the nano polypropylene acid absorption resin of sodium microballoon of relative vinylbenzene quality 0.3% is dissolved in the styrene monomer, mixing solutions is placed reactor, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 0.67%, 95 ℃ of set temperatures, 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, the free radical suspensioning polymerization stage initiator benzoyl peroxide amount that adds 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.Obtain water base polystyrene foamed, the good dispersity of water-absorbing resin microballoon in matrix, water content 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.
Example 15: at first, the nano polypropylene acid absorption resin of sodium microballoon of relative vinylbenzene quality 0.1% is dissolved in the styrene monomer, mixing solutions is placed reactor, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 0.67%, 95 ℃ of set temperatures, 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, the free radical suspensioning polymerization stage initiator benzoyl peroxide amount that adds 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.Obtain water base polystyrene foamed, the good dispersity of water-absorbing resin microballoon in matrix, water content 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 steeping in water for reconstitution foamed polystyrene is characterized in that step is as follows:
(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%, then the water soluble oxidized reduction initiator potassium persulfate that adds relative vinylformic acid quality 3%, the cyclohexane give that adds relative vinylformic acid quality 500% is external phase, the emulsifier span-80 that adds relative hexanaphthene quality 8%, the linking agent N of relative vinylformic acid quality 0.015%, the N-methylene-bisacrylamide, temperature of reaction is 75 ℃, stir speed (S.S.) 600-800rpm, N
2Lower polymerization 4-6 hour of condition protection then by azeotropic removal of water and external phase hexanaphthene, obtains flaxen product and is the absorption resin of sodium polyacrylate microballoon after the vacuum-drying;
(2) method that adopts free radical in-situ copolymerization and free radical suspensioning polymerization to combine prepares the steeping in water for reconstitution foamed polystyrene: at first, the nano polypropylene acid absorption resin of sodium microballoon that in styrene monomer, obtains in the step (1) of the relative vinylbenzene quality 0.1%-1% of dissolving, to the free radical in-situ copolymerization stage initiator benzoyl peroxide that wherein adds relative vinylbenzene quality 0.3%-1%, 95 ℃ of set temperatures, stir speed (S.S.) 800rpm, free 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, the free radical suspensioning polymerization stage initiator benzoyl peroxide that adds 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 polymerization finished, the filtration washing product namely got the steeping in water for reconstitution foamed polystyrene.
2. the preparation method of a kind of steeping in water for reconstitution foamed polystyrene 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 steeping in water for reconstitution foamed polystyrene according to claim 1 is characterized in that adding the free radical in-situ copolymerization stage initiator benzoyl peroxide of relative styrene monomer quality 0.67%.
4. the preparation method of a kind of steeping in water for reconstitution foamed polystyrene according to claim 1 is characterized in that the free radical in-situ copolymerization time is 1h.
5. the preparation method of a kind of steeping in water for reconstitution foamed polystyrene according to claim 1 is characterized in that adding the free radical suspensioning polymerization stage initiator benzoyl peroxide of relative styrene monomer quality 1%.
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| 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 |
| CN114875572B (en) * | 2021-05-21 | 2024-01-23 | 东莞市兆信电子科技有限公司 | Composite board with electromagnetic shielding performance |
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| 苯乙烯/聚丙烯酸钠原位聚合物的水崩解性研究;金峰等;《塑料工业》;20050531;第165-167，173页 * |
| 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》.2005,第165-167，173页. |
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