CN105504106A - Brominated polystyrene with high thermal stability and preparation method of brominated polystyrene - Google Patents
Brominated polystyrene with high thermal stability and preparation method of brominated polystyrene Download PDFInfo
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- CN105504106A CN105504106A CN201510978552.4A CN201510978552A CN105504106A CN 105504106 A CN105504106 A CN 105504106A CN 201510978552 A CN201510978552 A CN 201510978552A CN 105504106 A CN105504106 A CN 105504106A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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Abstract
The invention relates to the technical field of high-polymer brominated flame retardants, in particular to brominated polystyrene with high thermal stability and a preparation method of brominated polystyrene. Brominated polystyrene with the high thermal stability comprises raw materials including polystyrene, dichloroethane, antimony trichloride, bromine chloride and hot water. The thermal stability of brominated polystyrene can be improved, the 1% thermal weight loss temperature of brominated polystyrene is substantially increased, and the burning color is remarkably changed.
Description
Technical field
The present invention relates to polymer bromide fire retardant preparing technical field, be specifically related to a kind of high-heat stability bromized polystyrene and preparation method thereof.
Background technology
Flourish along with petroleum industry, the process for processing of macromolecular material also achieves significant progress, in daily life, little of a ballpoint pen, the large figure being invariably flooded with macromolecular material to refrigerator washing machine.Just because of the widespread use of macromolecular material, the attention rate of people to related products is also more and more higher, and the series of problems that causes related products (such as easily cause fire, combustionmaterial easily carcinogenic etc.) is also more and more concerned about.So, the requirement that the harmless high quality fire retardant of difficult combustion high-efficiency low-toxicity increases material day by day to meet people can be produced, become the target that each large enterprises and institute are competitively pursued.
In recent years, flourish along with Polymer Material Industry, its inflammableness is also more and more paid attention to by people, and as the functional aid reducing macromolecular material burning capacity, the ultimate production of whole world fire retardant is also just with stable speed sustainable growth.As a kind of additive flame retardant, brominated Polystyrene is widely used in nylon, polyethylene terephthalate, in the engineering plastics ignition resistant substrate such as polybutylene terephthalate.
Authorization Notice No. is the Chinese patent " preparation method of brominated polystyrene " of CN101701046B, and involved preparation method of brominated polystyrene comprises catalytic bromination, neutralization washing, solidification separation three steps.Catalytic bromination, polystyrene is dissolved in dichloroethane solvent, antimony trichloride catalyst is added in solution, bromine chloride is dripped gradually again in the solution adding antimony trichloride catalyst, bromine chloride and polystyrene monomers mol ratio are 3.8: 1 ~ 3.5: 1, under keeping temperature 10 DEG C ~ 25 DEG C conditions, react 3 ~ 4 hours; Neutralization washing, adds 5wt% S-WAT or aqueous solution of sodium bisulfite termination reaction in the polystyrene reactant liquid after catalytic bromination, then adds 5wt% sodium hydroxide solution to neutral, then washes with water; Solidification is separated, brominated Polystyrene solution after neutralization washing is added in the high-speed mixing equipment of the band high shear force filling separation of ethanol agent with the speed of 5mL/min ~ 20mL/min, adjusting rotary speed is at 2000 ~ 3000 turns of per minutes, brominated polystyrene product disperses in ethanol and is solidified into small-particle, refilter after isolating solid product washing with alcohol, dry, obtain brominated polystyrenic product.
Although the method technique is simple, be easy to scale operation, the brominated Polystyrene thermostability of gained is low, and color is partially yellow, limits its range of application.
Summary of the invention
The object of the invention is to solve the problem, a kind of high-heat stability bromized polystyrene and preparation method thereof is provided, can solve the problem.
The present invention's adopted technical scheme that solves the problem is:
A kind of high-heat stability bromized polystyrene, the raw material of described high-heat stability bromized polystyrene comprises polystyrene, ethylene dichloride, butter of antimony, bromine chloride and hot water.
Preferably, the consumption (mass fraction) of described raw material:
Polystyrene 20-30 part;
Ethylene dichloride 15-25 part;
Butter of antimony 1-5 part;
Bromine chloride 25-30 part;
Hot water 40-50 part.
Preferably, the consumption (mass fraction) of described raw material:
Polystyrene 25 parts;
Ethylene dichloride 20 parts;
Butter of antimony 3 parts;
Bromine chloride 28 parts;
Hot water 45 parts.
Preferably, the raw material of described bromine chloride comprises bromine, ethylene dichloride, chlorine.
Preferably, the consumption (mass fraction) of described raw material:
Bromine 10-15 part;
Ethylene dichloride 10-14 part;
Chlorine 1-5 part.
A preparation method for high-heat stability bromized polystyrene, carries out successively according to following step:
Step one: the bromine of certain mass number, ethylene dichloride are joined in stirred pot successively, the slowly chlorine of instillation certain mass number, obtained bromine chloride;
Step 2: be dissolved in ethylene dichloride by the polystyrene of certain mass number, carries out stirring according to certain rotating speed and makes it mutually dissolve;
Step 3: after dissolving, adds the butter of antimony of certain mass number;
Step 4: the bromine chloride at the uniform velocity adding above-mentioned mass fraction, ensures that the temperature of whole reaction system is maintained within a certain range;
Step 5: after adding, is incubated for some time at a certain temperature;
Step 6: neutralize with alkaline solution, washing;
Step 7: the hot water slowly adding certain temperature in above-mentioned solution, ensures that temperature out is maintained within a certain range, and can separate out product.
Preferably, the certain rotating speed described in step 2 is 600-700r/min.
Preferably, the certain limit described in step 4 is 50-60 DEG C.
Preferably, the certain temperature described in step 5 is 60 DEG C, and for some time is 3h.
Preferably, the certain temperature described in step 7 is 80-90 DEG C, and described certain limit is 82-85 DEG C.
The invention has the beneficial effects as follows: 1, the raw material of high-heat stability bromized polystyrene of the present invention comprises polystyrene, ethylene dichloride, butter of antimony, bromine chloride and hot water.Its thermal stability can be improved, increase substantially its 1% thermal weight loss temperature, the remarkable improvement of calcination color.
2, preparation method's production efficiency of the present invention is higher, more energy-conservation, not only can reduce recovery and the drying of ethylene dichloride, and the apparent colour obtained is whiter.Meanwhile, its thermal weight loss temperature of 1% is 371 DEG C, and 5% thermal weight loss temperature is 387 DEG C, and the calcination 10min of 300 DEG C still has good molten color.
Embodiment
Below by embodiment, the present invention is described in further detail:
Embodiment one
The preparation method of a kind of high-heat stability bromized polystyrene of the present invention, carries out successively according to the following step:
Step one: the bromine, the ethylene dichloride that mass fraction are respectively 10 parts, 10 parts join in stirred pot successively, slowly instillation mass fraction is the chlorine of 5 parts, obtained bromine chloride;
Step 2: be that to be dissolved in mass fraction be in the ethylene dichloride of 15 parts for the polystyrene of 20 parts by mass fraction is that 600r/min carries out stirring and makes it mutually dissolve according to rotating speed;
Step 3: after dissolving, adds the butter of antimony that mass fraction is 1 part;
Step 4: at the uniform velocity add the bromine chloride that mass fraction is 25 parts, ensures that the temperature of whole reaction system maintains 50 DEG C;
Step 5: after adding, is incubated 3h at 60 DEG C;
Step 6: neutralize with alkaline solution, washing;
Step 7: the hot water slowly adding 80 DEG C in above-mentioned solution, ensures that temperature out maintains 82 DEG C, can separate out product.
Embodiment two
Compared with embodiment one, in step one, the mass fraction of bromine is 13 parts, and the mass fraction of ethylene dichloride is 12 parts, and the mass fraction of chlorine is 3 parts; In step 2, the mass fraction of polystyrene is 25 parts, and the mass fraction of ethylene dichloride is 20 parts, and rotating speed is 650r/min; In step 3, the mass fraction of butter of antimony is 3 parts; In step 4, the mass fraction of bromine chloride is 28 parts, and temperature maintains 55 DEG C; Add the hot water of 85 DEG C in step 7, temperature maintains 83 DEG C.Other technical process is identical with embodiment one.
Embodiment three
Compared with embodiment one, in step one, the mass fraction of bromine is 15 parts, and the mass fraction of ethylene dichloride is 14 parts, and the mass fraction of chlorine is 1 part; In step 2, the mass fraction of polystyrene is 30 parts, and the mass fraction of ethylene dichloride is 25 parts, and rotating speed is 700r/min; In step 3, the mass fraction of butter of antimony is 5 parts; In step 4, the mass fraction of bromine chloride is 30 parts, and temperature maintains 60 DEG C; Add the hot water of 90 DEG C in step 7, temperature maintains 85 DEG C.Other technical process is identical with embodiment one.
The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (10)
1. a high-heat stability bromized polystyrene, is characterized in that: the raw material of described high-heat stability bromized polystyrene comprises polystyrene, ethylene dichloride, butter of antimony, bromine chloride and hot water.
2. a kind of high-heat stability bromized polystyrene according to claim 1, is characterized in that: the consumption (mass fraction) of described raw material:
Polystyrene 20-30 part;
Ethylene dichloride 15-25 part;
Butter of antimony 1-5 part;
Bromine chloride 25-30 part;
Hot water 40-50 part.
3. a kind of high-heat stability bromized polystyrene according to claim 2, is characterized in that: the consumption (mass fraction) of described raw material:
Polystyrene 25 parts;
Ethylene dichloride 20 parts;
Butter of antimony 3 parts;
Bromine chloride 28 parts;
Hot water 45 parts.
4. a kind of high-heat stability bromized polystyrene according to claim 1, is characterized in that: the raw material of described bromine chloride comprises bromine, ethylene dichloride, chlorine.
5. a kind of high-heat stability bromized polystyrene according to claim 4, is characterized in that: the consumption (mass fraction) of described raw material:
Bromine 10-15 part;
Ethylene dichloride 10-14 part;
Chlorine 1-5 part.
6. prepare a method for the high-heat stability bromized polystyrene described in claim 1-5, it is characterized in that: carry out successively according to following step:
Step one: the bromine of certain mass number, ethylene dichloride are joined in stirred pot successively, the slowly chlorine of instillation certain mass number, obtained bromine chloride;
Step 2: be dissolved in ethylene dichloride by the polystyrene of certain mass number, carries out stirring according to certain rotating speed and makes it mutually dissolve;
Step 3: after dissolving, adds the butter of antimony of certain mass number;
Step 4: the bromine chloride at the uniform velocity adding above-mentioned mass fraction, ensures that the temperature of whole reaction system is maintained within a certain range;
Step 5: after adding, is incubated for some time at a certain temperature;
Step 6: neutralize with alkaline solution, washing;
Step 7: the hot water slowly adding certain temperature in above-mentioned solution, ensures that temperature out is maintained within a certain range, and can separate out product.
7. the preparation method of a kind of high-heat stability bromized polystyrene according to claim 6, is characterized in that: the certain rotating speed described in step 2 is 600-700r/min.
8. the preparation method of a kind of high-heat stability bromized polystyrene according to claim 6, is characterized in that: the certain limit described in step 4 is 50-60 DEG C.
9. the preparation method of a kind of high-heat stability bromized polystyrene according to claim 6, is characterized in that: the certain temperature described in step 5 is 60 DEG C, and for some time is 3h.
10. the preparation method of a kind of high-heat stability bromized polystyrene according to claim 6, is characterized in that: the certain temperature described in step 7 is 80-90 DEG C, and described certain limit is 82-85 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107474165A (en) * | 2017-08-03 | 2017-12-15 | 山东日兴新材料股份有限公司 | A kind of high-heat stability bromized SBS synthetic method |
| CN117247482A (en) * | 2023-11-17 | 2023-12-19 | 山东旭锐新材股份有限公司 | High-thermal-stability brominated polystyrene synthesis method |
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| CN1275992A (en) * | 1997-11-18 | 2000-12-06 | 费罗公司 | Process for the preparation of brominated polystyrene having improved color characteristics |
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| CN102504067A (en) * | 2011-10-26 | 2012-06-20 | 山东润科化工股份有限公司 | Method for preparing bromination polystyrene |
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2015
- 2015-12-24 CN CN201510978552.4A patent/CN105504106A/en active Pending
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| EP0020294A1 (en) * | 1979-05-07 | 1980-12-10 | Ciba-Geigy Ag | A process for the preparation of brominated products of polystyrene |
| CN1275992A (en) * | 1997-11-18 | 2000-12-06 | 费罗公司 | Process for the preparation of brominated polystyrene having improved color characteristics |
| CN101319017A (en) * | 2008-07-23 | 2008-12-10 | 天津长芦海晶集团有限公司 | Method of preparing high-heat stability bromized polystyrene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107474165A (en) * | 2017-08-03 | 2017-12-15 | 山东日兴新材料股份有限公司 | A kind of high-heat stability bromized SBS synthetic method |
| CN117247482A (en) * | 2023-11-17 | 2023-12-19 | 山东旭锐新材股份有限公司 | High-thermal-stability brominated polystyrene synthesis method |
| CN117247482B (en) * | 2023-11-17 | 2024-02-20 | 山东旭锐新材股份有限公司 | High-thermal-stability brominated polystyrene synthesis method |
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Application publication date: 20160420 |