CN101633709B - Method for preparing colorful polystyrene particle synthesized by in-situ suspension polymerization one-step process - Google Patents
Method for preparing colorful polystyrene particle synthesized by in-situ suspension polymerization one-step process Download PDFInfo
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Abstract
The invention relates to a method for preparing colorful polystyrene particles that are synthesized by an in-situ suspension polymerization one-step process. The method comprises two parts: in-situ modification of inorganic pigment and synthesis of colorful polystyrene particles; de-ionized water, surfactant, dispersant and anhydrous sodium sulfate solution are in turn added in a four-neck flask and evenly stirred, then styrene monomer, butyl acrylate, oil-based nanometer inorganic pigment paste and initiator are in turn added in the four-neck flask, after the particles are cured and hardened, the mixture is stopped heating and cooled to discharge, the obtained particles are washed with acid solution and de-ionized water and then dried at room temperature to obtain the colorful polystyrene particles. The invention realizes the molecular coating of inorganic particles and avoids such problem as poor compatibility between inorganic pigment and polymer during the blending, extrusion and granulation processes. The prepared colorful polystyrene particles have controllable colors and uniform grain diameters; the preparation process of the colorful polystyrene particles is simplified; and the invention has the advantages of low reaction temperature, simple process, easy operation, environmentally-friendly and low cost.
Description
Technical field
The invention belongs to the preparation and the application of matrix material, especially relate to the preparation of the colorful polystyrene particle of uniform particle diameter, controllable color.
Background technology
Along with the domestic and international market is increasingly competitive, increase along with field p-poly-phenyl vinyl material demands such as industry, building trade and daily lifes, along with the expansion of Expandable Polystyrene (EPS) product application, the Expandable Polystyrene (EPS) product is just towards multi-functional, and the high-performance direction develops.Colorful polystyrene particle is at casing for electric appliances injection moulding pellet; The building and ornament materials pellet; Stationery material pellet; Pipe material pellet; The automotive upholstery pellet; Expandable Polystyrene (EPS) belongs to exotic materials with widespread use in the fields such as pellet.The present domestic technology that does not also have single stage method to prepare colorful polystyrene particle.
At present, in the preparation of chromogen bonded polymer particle, mainly be to adopt polymkeric substance and pigment particles blend extruding pelletization, but because pigment particles specific physical character, pigment particle size is little, and surface energy is bigger, is easy to reunite, be difficult in polymeric matrix, be uniformly dispersed, be difficult to obtain ideal chromogen bonded polymer particle.And consistency is relatively poor between pigment and the polymkeric substance, has influenced the mechanical property of polymkeric substance.Another method is to carry out colored application after the polymer particle extrusion molding, and this method shortcoming is that the inside of moulding product will be exposed in a single day the surface is scratched after, and this scratch position will show money or valuables one carries unintentionally; And, also increased this procedure of application, so will increase its cost, purposes also can be restricted.
Summary of the invention
Purpose of the present invention just is at above-mentioned the deficiencies in the prior art, and a kind of preparation method of in-situ suspension polymerization single stage method synthetic colorful polystyrene particle is provided.
The objective of the invention is to be achieved through the following technical solutions:
The preparation method of in-situ suspension polymerization single stage method synthetic colorful polystyrene particle comprises following order and step:
The in-situ modification of mineral dye:
Inorganic nano pigment 0.3～1.5 is restrained ultra-sonic dispersion in 100 ml distilled waters, in sand mill, ground then 20～30 minutes, transfer in the four-hole bottle that has mechanicalness stirring and prolong, stirring velocity is 200～400 rev/mins and is heated to 60 ℃, drips oleic acid 0.2～1.3 gram, be warming up to 80 ℃, reacted 30～50 minutes, and stopped heating and stir, with 5～20 milliliters of carrier fluid extracting and separating, ultra-sonic dispersion obtains stable oil base nano inorganic pigment slurry, places standby.
Synthesizing of colorful polystyrene particle:
A, in having the four-hole bottle that prolong and mechanical type stir, add deionized water 400～550% successively and (press the per-cent of styrene monomer quality, below express identical), concentration is that 0.02% aqueous solution of anionic surfactant 30～80%, inorganic main dispersant 0.5～2%, inorganic auxiliary dispersants 1～2.5% and concentration are 4% the organic dispersing agent aqueous solution 30～70%, the mechanical stirring rotating speed is 180～320 rev/mins, pre-dispersed 10～20 minutes;
B, with monomer styrene 100%; Toughness reinforcing comonomer acrylate 5～30%; Oil base nano inorganic pigment slurry 5～40%; Initiator 0.5～2% joins successively and has in mechanicalness stirring and the prolong four-hole bottle, continue to stir, slowly heating up in 70～100 minutes then is 79～83 ℃, add inorganic main dispersant 0.5～2% this moment, add inorganic main dispersant 0.5～2% after 1 hour once more, splash in the beaker of containing distilled water with the continuous sampling of stopple coupon in the reaction process, observe the growing way of particle, regulate size by adding inorganic main dispersant, 2.5 the sampling particle sank in～4 hours, add inorganic main dispersant 0.5～2% once more, continue reaction and made particle slaking hardening in 2～4 hours, stop heating and be cooled to 10～30 ℃ of dischargings.
C, with the particle concentration for preparing be 5～15% diluted hydrochloric acid aqueous solutions and deionized water rinsing repeatedly, room temperature is dried, and obtains colorful polystyrene particle, calculates productive rate
Purpose of the present invention can also be achieved through the following technical solutions:
Employed tensio-active agent is any in anionic surfactant sodium dodecylbenzene sulfonate or the sodium lauryl sulphate; Wherein inorganic main dispersant is any in active calcium phosphate, magnesiumcarbonate, barium sulfate, talcum powder or the kaolin; Inorganic auxiliary dispersants be in anhydrous sodium sulphate or the sodium pyrosulfate any; Organic dispersing agent be in polyvinyl alcohol, gelatin or the carboxymethyl cellulose any; The extracting and separating carrier fluid of mineral dye is selected any in methyl methacrylate or the vinylbenzene for use behind the in-situ modification; Oil base nano inorganic pigment slurry is Fe
3O
4, Hua Lan, iron oxide red, illusion-colour is dark green, illusion-colour is greenish-yellow, in permanent violet or the pearl purple any; Initiator is benzoyl peroxide or Diisopropyl azodicarboxylate; The toughness reinforcing comonomer acrylate that uses be in butyl acrylate, ethyl propenoate or the Ethyl acrylate any.
Beneficial effect of the present invention is: utilize oleic acid that inorganic nano pigment is carried out in-situ modification, obtain the lipophilic nano mineral dye, utilize carrier fluid methyl methacrylate or vinylbenzene that mineral dye is carried out extracting and separating simultaneously, obtain finely dispersed oil base nano inorganic pigment slurry like this.Then, in the styrene suspension polymerization process, add above-mentioned oil base nano inorganic pigment slurry, make oil base nano inorganic pigment slurry can be dispersed in the monomer like this, in polymerization process, realize coating the inorganic particulate molecular level.Avoided relatively poor this defect problem of consistency between inorganic particulate and the polymkeric substance, and control the color of compound particle by the add-on of regulating oil base nano inorganic pigment slurry, also can regulate toughening effect simultaneously, solve the deficiency of each method existence in the past by the add-on that changes toughness reinforcing comonomer acrylate.The in-situ suspension polymerization single stage method is synthesized colorful polystyrene particle, has not only avoided this relatively poor defect problem of consistency between mineral dye and the polymkeric substance in the technological process, and has simplified colorful polystyrene particle preparation technology.Preparation method of the present invention adopts water to do reaction medium, and cheap dispersion agent is done polymerization protection system, and temperature of reaction is lower, and technology is simple, and is easy to operate, environmentally friendly, and cost is lower, and Application Areas is extensive.
Description of drawings
Fig. 1. different oil base Fe
3O
4The colorful polystyrene particle photo that the pigment slurry add-on prepares
Fig. 2. the colorful polystyrene particle photo that adding oil base Hua Lan, oil base iron oxide red pigment slurry prepare
Fig. 3. add the colorful polystyrene particle photo that the dark green pigment slurry of oil base illusion-colour prepares
Embodiment
Be described in further detail below in conjunction with embodiment:
Embodiment 1:
The in-situ modification of mineral dye:
With inorganic nano pigment Fe
3O
40.5 the gram ultra-sonic dispersion is in 100 ml distilled waters, in sand mill, ground 20 minutes then, transfer in the four-hole bottle that has mechanicalness stirring and prolong, stirring velocity is 300 rev/mins and is heated to 60 ℃, drips oleic acid 0.6 gram, is warming up to 80 ℃, react after 35 minutes, stop heating and stir, with 15 milliliters of methyl methacrylate extracting and separating, ultra-sonic dispersion obtains stable oil base nanometer Fe then
3O
4Pigment slurry is placed standby.
Synthesizing of colorful polystyrene particle:
A, to add 45 ml deionized water, 0.07 gram active calcium phosphate, 0.15 gram anhydrous sodium sulphate, concentration successively in having the four-hole bottle that prolong and mechanical type stir be that 0.02% 4 milliliters of sodium dodecyl benzene sulfonate aqueous solutions and concentration are 3.5 milliliters of 4% polyvinyl alcohol water solutions, the mechanical stirring rotating speed is 200 rev/mins, pre-dispersed 10 minutes;
B, in four-hole bottle, add styrene monomer 10 gram, toughness reinforcing comonomer butyl acrylate 1 gram, oil base nanometer Fe successively
3O
4 Pigment slurry 1 gram and benzoyl peroxide 0.12 gram, slowly heated up 90 minutes to 81 ℃, add 0.05 gram active calcium phosphate this moment, add 0.1 gram active calcium phosphate after 1 hour once more, splash in the beaker of containing distilled water with the continuous sampling of stopple coupon in the reaction process, observe the growing way of particle, regulate size by adding active calcium phosphate, after the particle sinking is observed in sampling after 3 hours, add 0.05 gram active calcium phosphate once more, continue reaction and made particle slaking hardening in 3 hours, stop heating and be cooled to 30 ℃ of dischargings;
C, with the particle concentration for preparing be 10% dilute hydrochloric acid solution and deionized water rinsing repeatedly, room temperature is dried, the colorful polystyrene particle (seeing Fig. 1 .A) that obtains uniform particle diameter and have magnetic, calculating productive rate is 96%.
Embodiment 2:
The in-situ modification of mineral dye:
With inorganic nano pigment Fe
3O
40.5 the gram ultra-sonic dispersion is in 100 ml distilled waters, in sand mill, ground 20 minutes then, transfer in the four-hole bottle that has mechanicalness stirring and prolong, stirring velocity is 300 rev/mins and is heated to 60 ℃, drips oleic acid 0.6 gram, is warming up to 80 ℃, react after 35 minutes, stop heating and stir, with 15 milliliters of methyl methacrylate extracting and separating, ultra-sonic dispersion obtains stable oil base nanometer Fe then
3O
4Pigment slurry is placed standby.
Synthesizing of colorful polystyrene particle:
A, to add 45 ml deionized water, 0.07 gram talcum powder, 0.13 gram anhydrous sodium sulphate, concentration successively in having the four-hole bottle that prolong and mechanical type stir be that 0.02% 5 milliliters of lauryl sodium sulfate aqueous solution and concentration are 4 milliliters of 4% polyvinyl alcohol water solutions, the mechanical stirring rotating speed is 180 rev/mins, pre-dispersed 10 minutes;
B, in four-hole bottle, add styrene monomer 10 gram, toughness reinforcing comonomer ethyl propenoate 1 gram, oil base nanometer Fe successively
3O
4 Pigment slurry 2 grams and Diisopropyl azodicarboxylate 0.12 gram, slowly heated up 80 minutes to 80 ℃, add 0.10 gram talcum powder this moment, add 0.10 gram talcum powder after 1 hour once more, splash in the beaker of containing distilled water with the continuous sampling of stopple coupon in the reaction process, observe the growing way of particle, regulate size by adding talcum powder, after the particle sinking is observed in sampling after 3 hours, add 0.06 gram talcum powder once more, continue reaction and made particle slaking hardening in 3 hours, stop heating and be cooled to 10 ℃ of dischargings;
C, with the particle concentration for preparing be 15% dilute hydrochloric acid solution and deionized water rinsing repeatedly, room temperature is dried, the colorful polystyrene particle (seeing Fig. 1 .B) that obtains uniform particle diameter and have magnetic, calculating productive rate is 95%.
Embodiment 3:
The in-situ modification of mineral dye:
With inorganic nano pigment Fe
3O
40.5 the gram ultra-sonic dispersion is in 100 ml distilled waters, in sand mill, ground 20 minutes then, transfer in the four-hole bottle that has mechanicalness stirring and prolong, stirring velocity is 300 rev/mins and is heated to 60 ℃, drips oleic acid 0.6 gram, is warming up to 80 ℃, react after 35 minutes, stop heating and stir, with 15 milliliters of vinylbenzene extracting and separating, ultra-sonic dispersion obtains stable oil base nanometer Fe then
3O
4Pigment slurry is placed standby.
Synthesizing of colorful polystyrene particle:
A, to add 45 ml deionized water, 0.07 gram magnesiumcarbonate, 0.16 gram anhydrous sodium sulphate, concentration successively in having the four-hole bottle that prolong and mechanical type stir be that 0.02% 5 milliliters of sodium dodecyl benzene sulfonate aqueous solutions and concentration are 5 milliliters of 4% aqueous gelatin solutions, the mechanical stirring rotating speed is 200 rev/mins, pre-dispersed 10 minutes;
B, in four-hole bottle, add styrene monomer 10 gram, toughness reinforcing comonomer butyl acrylate 1 gram, oil base nanometer Fe successively
3O
4 Pigment slurry 3 grams and Diisopropyl azodicarboxylate 0.12 gram, slowly heated up 70 minutes to 79 ℃, add 0.15 gram magnesiumcarbonate this moment, add 0.1 gram magnesiumcarbonate after 1 hour once more, splash in the beaker of containing distilled water with the continuous sampling of stopple coupon in the reaction process, observe the growing way of particle, regulate size by adding magnesiumcarbonate, after the particle sinking is observed in sampling after 3 hours, add 0.06 gram magnesiumcarbonate once more, continue reaction and made particle slaking hardening in 3 hours, stop heating and be cooled to 20 ℃ of dischargings;
C, with the particle concentration for preparing be 12% dilute hydrochloric acid solution and deionized water rinsing repeatedly, room temperature is dried, the colorful polystyrene particle (seeing Fig. 1 .C) that obtains uniform particle diameter and have magnetic, calculating productive rate is 98%.
Embodiment 4:
The in-situ modification of mineral dye:
With inorganic nano pigment Fe
3O
40.5 the gram ultra-sonic dispersion is in 100 ml distilled waters, in sand mill, ground 20 minutes then, transfer in the four-hole bottle that has mechanicalness stirring and prolong, stirring velocity is 300 rev/mins and is heated to 60 ℃, drips oleic acid 0.6 gram, is warming up to 80 ℃, react after 35 minutes, stop heating and stir, with 15 milliliters of vinylbenzene extracting and separating, ultra-sonic dispersion obtains stable oil base nanometer Fe then
3O
4Pigment slurry is placed standby.
Synthesizing of colorful polystyrene particle:
A, to add 45 ml deionized water, 0.07 gram active calcium phosphate, 0.17 gram anhydrous sodium sulphate, concentration successively in having the four-hole bottle that prolong and mechanical type stir be that 0.02% 4 milliliters of lauryl sodium sulfate aqueous solution and concentration are 5 milliliters of 4% polyvinyl alcohol water solutions, the mechanical stirring rotating speed is 240 rev/mins, pre-dispersed 10 minutes;
B, in four-hole bottle, add styrene monomer 10 gram, toughness reinforcing comonomer Ethyl acrylate 1 gram, oil base nanometer Fe successively
3O
4 Pigment slurry 4 grams and benzoyl peroxide 0.12 gram, slowly heated up 85 minutes to 80 ℃, add 0.15 gram active calcium phosphate this moment, add 0.1 gram active calcium phosphate after 1 hour once more, splash in the beaker of containing distilled water with the continuous sampling of stopple coupon in the reaction process, observe the growing way of particle, regulate size by adding active calcium phosphate, after the particle sinking is observed in sampling after 3 hours, add 0.1 gram active calcium phosphate once more, continue reaction and made particle slaking hardening in 3 hours, stop heating and be cooled to 15 ℃ of dischargings;
C, with the particle concentration for preparing be 8% dilute hydrochloric acid solution and deionized water rinsing repeatedly, room temperature is dried, the colorful polystyrene particle (seeing Fig. 1 .D) that obtains uniform particle diameter and have magnetic, calculating productive rate is 98%.
Embodiment 5:
The in-situ modification of mineral dye:
Inorganic nano pigment China blue 0.5 is restrained ultra-sonic dispersion in 100 ml distilled waters, in sand mill, ground 30 minutes then, transfer in the four-hole bottle that has mechanicalness stirring and prolong, stirring velocity is 350 rev/mins and is heated to 60 ℃, drips oleic acid 0.8 gram, be warming up to 80 ℃, react after 50 minutes, stop heating and stir, with 10 milliliters of methyl methacrylate extracting and separating, ultra-sonic dispersion obtains the stable blue pigment slurry of oil base nanometer China then, places standby.
Synthesizing of colorful polystyrene particle:
A, to add 45 ml deionized water, 0.07 gram kaolin, 0.13 gram anhydrous sodium sulphate, concentration successively in having the four-hole bottle that prolong and mechanical type stir be that 0.02% 5 milliliters of sodium dodecyl benzene sulfonate aqueous solutions and concentration are 4 milliliters of 4% polyvinyl alcohol water solutions, the mechanical stirring rotating speed is 260 rev/mins, pre-dispersed 10 minutes;
B, in four-hole bottle, add styrene monomer 10 grams successively, toughness reinforcing comonomer butyl acrylate 1 gram, blue pigment slurry 3 grams of oil base nanometer China and Diisopropyl azodicarboxylate 0.12 gram, slowly heated up 100 minutes to 82 ℃, add 0.05 gram kaolin this moment, add 0.1 gram kaolin after 1 hour once more, splash in the beaker of containing distilled water with the continuous sampling of stopple coupon in the reaction process, observe the growing way of particle, regulate size by adding kaolin, after the particle sinking is observed in sampling after 3 hours, add 0.1 gram kaolin once more, continue reaction and made particle slaking hardening in 3 hours, stop heating and be cooled to 20 ℃ of dischargings;
C, with the particle concentration for preparing be 12% dilute hydrochloric acid solution and deionized water rinsing repeatedly, room temperature is dried, and obtains the colorful polystyrene particle (seeing Fig. 2 .E) of uniform particle diameter, calculating productive rate is 95%.
Embodiment 6:
The in-situ modification of mineral dye:
Inorganic nano pigment iron oxide red 0.5 is restrained ultra-sonic dispersion in 100 ml distilled waters, in sand mill, ground 30 minutes then, transfer in the four-hole bottle that has mechanicalness stirring and prolong, stirring velocity is 380 rev/mins and is heated to 60 ℃, drips oleic acid 0.7 gram, be warming up to 80 ℃, react after 40 minutes, stop heating and stir, with 13 milliliters of vinylbenzene extracting and separating, ultra-sonic dispersion obtains stable oil base nanometer iron oxide red pigment slurry then, places standby.
Synthesizing of colorful polystyrene particle:
A, to add 45 ml deionized water, 0.07 gram barium sulfate, 0.15 gram anhydrous sodium sulphate, concentration successively in having the four-hole bottle that prolong and mechanical type stir be that 0.02% 4 milliliters of lauryl sodium sulfate aqueous solution and concentration are 4 milliliters of 4% aqueous gelatin solutions, the mechanical stirring rotating speed is 320 rev/mins, pre-dispersed 10 minutes;
B, in four-hole bottle, add styrene monomer 10 grams successively, toughness reinforcing comonomer Ethyl acrylate 1 gram, oil base nanometer iron oxide red pigment slurry 1 gram and Diisopropyl azodicarboxylate 0.12 gram, slowly heated up 90 minutes to 83 ℃, add 0.1 gram barium sulfate this moment, add 0.05 gram barium sulfate after 1 hour once more, splash in the beaker of containing distilled water with the continuous sampling of stopple coupon in the reaction process, observe the growing way of particle, regulate size by adding barium sulfate, after the particle sinking is observed in sampling after 3 hours, add 0.05 gram activared carbon sulfur barium once more, continue reaction and made particle slaking hardening in 3 hours, stop heating and be cooled to 25 ℃ of dischargings;
C, with the particle concentration for preparing be 7% dilute hydrochloric acid solution and deionized water rinsing repeatedly, room temperature is dried, and obtains the colorful polystyrene particle (seeing Fig. 2 .F) of uniform particle diameter, calculating productive rate is 97%.
Embodiment 7:
The in-situ modification of mineral dye:
Inorganic nano pigment illusion-colour dark green 0.5 is restrained ultra-sonic dispersion in 100 ml distilled waters, in sand mill, ground 30 minutes then, transfer in the four-hole bottle that has mechanicalness stirring and prolong, stirring velocity is 380 rev/mins and is heated to 60 ℃, drips oleic acid 0.4 gram, be warming up to 80 ℃, react after 40 minutes, stop heating and stir, with 10 milliliters of methyl methacrylate extracting and separating, ultra-sonic dispersion obtains the stable dark green pigment slurry of oil base nanometer illusion-colour then, places standby.
Synthesizing of colorful polystyrene particle:
A, to add 45 ml deionized water, 0.07 gram active calcium phosphate, 0.15 gram anhydrous sodium sulphate, concentration successively in having the four-hole bottle that prolong and mechanical type stir be that 0.02% 4 milliliters of sodium dodecyl benzene sulfonate aqueous solutions and concentration are 3.5 milliliters of 4% carboxymethyl cellulose aqueous solutions, the mechanical stirring rotating speed is 320 rev/mins, pre-dispersed 10 minutes;
B, in four-hole bottle, add styrene monomer 10 grams successively, toughness reinforcing comonomer butyl acrylate 1 gram, dark green pigment slurry 2 grams of oil base nanometer illusion-colour and benzoyl peroxide 0.12 gram, slowly heated up 90 minutes to 83 ℃, add 0.1 gram active calcium phosphate this moment, add 0.1 gram active calcium phosphate after 1 hour once more, splash in the beaker of containing distilled water with the continuous sampling of stopple coupon in the reaction process, observe the growing way of particle, regulate size by adding active calcium phosphate, after the particle sinking is observed in sampling after 3 hours, add 0.1 gram active calcium phosphate once more, continue reaction and made particle slaking hardening in 3 hours, stop heating and be cooled to 30 ℃ of dischargings;
C, with the particle concentration for preparing be 5% dilute hydrochloric acid solution and deionized water rinsing repeatedly, room temperature is dried, and obtains the colorful polystyrene particle (seeing Fig. 3 .G) of uniform particle diameter, calculating productive rate is 95%.
Claims (7)
1. the preparation method of in-situ suspension polymerization single stage method synthetic colorful polystyrene particle is characterized in that, comprises following order and step:
---the in-situ modification of mineral dye:
Inorganic nano pigment 0.3～1.5 is restrained ultra-sonic dispersion in 100 ml distilled waters, in sand mill, ground then 20～30 minutes, transfer in the four-hole bottle that has mechanicalness stirring and prolong, stirring velocity is 200～400 rev/mins and is heated to 60 ℃, drips oleic acid 0.2～1.3 gram, be warming up to 80 ℃, reacted 30～50 minutes, and stopped heating and stir, with 5～20 milliliters of carrier fluid extracting and separating, ultra-sonic dispersion obtains stable oil base nano inorganic pigment slurry, places standby;
---synthesizing of colorful polystyrene particle:
A, to add deionized water 400～550%, concentration by the styrene monomer mass percent successively in having the four-hole bottle that prolong and mechanical type stir be that 0.02% aqueous solution of anionic surfactant 30～80%, inorganic main dispersant 0.5～2%, inorganic auxiliary dispersants 1～2.5% and concentration are 4% the organic dispersing agent aqueous solution 30～70%, the mechanical stirring rotating speed is 180～320 rev/mins, pre-dispersed 10～20 minutes;
B, with monomer styrene 100%; Toughness reinforcing comonomer acrylate 5～30%; Oil base nano inorganic pigment slurry 5～40%; Initiator 0.5～2% joins successively and has in mechanicalness stirring and the prolong four-hole bottle, continue to stir, slowly heating up in 70～100 minutes then is 79～83 ℃, add inorganic main dispersant 0.5～2% this moment, add inorganic main dispersant 0.5～2% after 1 hour once more, splash in the beaker of containing distilled water with the continuous sampling of stopple coupon in the reaction process, observe the growing way of particle, regulate size by adding inorganic main dispersant, 2.5 the sampling particle sank in～4 hours, add inorganic main dispersant 0.5～2% once more, continue reaction and made particle slaking hardening in 2～4 hours, stop heating and be cooled to 10～30 ℃ of dischargings;
C, with the particle concentration for preparing be 5～15% diluted hydrochloric acid aqueous solutions and deionized water rinsing repeatedly, room temperature is dried, and obtains colorful polystyrene particle, calculates productive rate:
2. according to the preparation method of right 1 described in-situ suspension polymerization single stage method synthetic colorful polystyrene particle, it is characterized in that the anion surfactant of use can be any in Sodium dodecylbenzene sulfonate or the sodium lauryl sulphate.
3. according to the preparation method of right 1 described in-situ suspension polymerization single stage method synthetic colorful polystyrene particle, it is characterized in that mineral dye is Fe
3O
4, Hua Lan, iron oxide red, illusion-colour is dark green, illusion-colour is greenish-yellow, in permanent violet or the pearl purple any.
4. according to the preparation method of right 1 described in-situ suspension polymerization single stage method synthetic colorful polystyrene particle, it is characterized in that the extracting and separating carrier fluid of the mineral dye that the oleic acid in-situ modification is crossed is methyl methacrylate or vinylbenzene.
5. according to the preparation method of right 1 described in-situ suspension polymerization single stage method synthetic colorful polystyrene particle, it is characterized in that, the dispersion agent that uses is a ternary composite dispersing agent system, wherein inorganic main dispersant is any in active calcium phosphate, magnesiumcarbonate, barium sulfate, talcum powder or the kaolin, inorganic auxiliary dispersants be in anhydrous sodium sulphate or the sodium pyrosulfate any; Organic dispersing agent be in polyvinyl alcohol, gelatin or the methylcellulose gum any.
6. according to the preparation method of right 1 described in-situ suspension polymerization single stage method synthetic colorful polystyrene particle, it is characterized in that initiator is benzoyl peroxide or Diisopropyl azodicarboxylate.
7. according to the preparation method of right 1 described in-situ suspension polymerization single stage method synthetic colorful polystyrene particle, it is characterized in that, the toughness reinforcing comonomer acrylate of use be in butyl acrylate, ethyl propenoate or the Ethyl acrylate any.
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| CN104530288B (en) * | 2014-12-22 | 2017-10-31 | 常熟市环虹化工颜料厂 | A kind of method of regulation and control microcapsules pigment particle size |
| CN107474166B (en) * | 2015-09-18 | 2019-10-18 | 武汉轻工大学 | A kind of polystyrene silver gray thermal insulation material preparation method of mica titanium filling in situ |
| CN105237661B (en) * | 2015-10-30 | 2017-06-09 | 武汉轻工大学 | The inhibition that disappears and the synthetic method of synchronous fire-retardant graphite polystyrene material |
| CN109251435B (en) * | 2018-09-21 | 2021-05-28 | 武汉轻工大学 | Colored polymer conductive bead and preparation method thereof |
| CN110982096B (en) * | 2019-12-27 | 2022-06-28 | 广东美联新材料股份有限公司 | Color master batch prepared based on in-situ polymerization of active monomer and preparation method thereof |
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