CN115636888A - Post-treatment method for brominated polystyrene - Google Patents
Post-treatment method for brominated polystyrene Download PDFInfo
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- CN115636888A CN115636888A CN202211670260.0A CN202211670260A CN115636888A CN 115636888 A CN115636888 A CN 115636888A CN 202211670260 A CN202211670260 A CN 202211670260A CN 115636888 A CN115636888 A CN 115636888A
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- 239000004793 Polystyrene Substances 0.000 title claims abstract description 63
- 229920002223 polystyrene Polymers 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000000047 product Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000012074 organic phase Substances 0.000 claims abstract description 27
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims abstract description 26
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 24
- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000007868 Raney catalyst Substances 0.000 claims abstract description 12
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000564 Raney nickel Inorganic materials 0.000 claims abstract description 12
- 239000012043 crude product Substances 0.000 claims abstract description 11
- 238000009835 boiling Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000001704 evaporation Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 230000007935 neutral effect Effects 0.000 claims abstract description 10
- 238000004321 preservation Methods 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000002425 crystallisation Methods 0.000 claims abstract description 3
- 230000008025 crystallization Effects 0.000 claims abstract description 3
- 230000008020 evaporation Effects 0.000 claims abstract description 3
- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 239000012071 phase Substances 0.000 claims description 9
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- MFRIHAYPQRLWNB-UHFFFAOYSA-N sodium tert-butoxide Chemical compound [Na+].CC(C)(C)[O-] MFRIHAYPQRLWNB-UHFFFAOYSA-N 0.000 claims description 6
- 230000004580 weight loss Effects 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 4
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 3
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 13
- 150000002431 hydrogen Chemical class 0.000 abstract description 5
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 5
- 125000003011 styrenyl group Chemical class [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000000379 polymerizing effect Effects 0.000 description 3
- 238000005893 bromination reaction Methods 0.000 description 2
- 150000004678 hydrides Chemical class 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000031709 bromination Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 239000012433 hydrogen halide Substances 0.000 description 1
- 229910000039 hydrogen halide Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a post-treatment method of brominated polystyrene, belonging to the technical field of post-treatment of high molecular polymers. Preparing a brominated polystyrene crude product into a solution by using a solvent, adding Raney nickel and an alkali source into the solution in a hydrogen atmosphere, continuously adding hydrogen, regulating the pressure to 0.1-1MPa, and preserving the temperature at 25-50 ℃ for 0.5-5h; and after the heat preservation is finished, washing the reaction finishing liquid to be neutral, separating out an organic phase, dripping the organic phase into boiling water for evaporation and crystallization, and filtering and drying to obtain a refined brominated polystyrene product. The post-treatment method of brominated polystyrene has mild reaction conditions and simple operation, and can realize selective hydrogenation to remove bromine on the main chain of the brominated polystyrene, thereby improving the thermal stability and whiteness of the brominated polystyrene.
Description
Technical Field
The invention belongs to the technical field of post-treatment of high molecular polymers, and particularly relates to a post-treatment method of brominated polystyrene.
Background
The industrial process for synthesizing brominated polystyrene mainly includes two technological routes of firstly brominating and then polymerizing polybrominated styrene and firstly polymerizing and then brominating brominated polystyrene. U.S. patent document No. US005369202A discloses a method for synthesizing brominated and polymerized polybrominated styrene, which avoids the halogenation reaction of a brominating agent on the main chain, so that the prepared polybrominated styrene has excellent thermal stability, and when the polybrominated styrene is used as a flame retardant and is melt blended with a flame-retardant base material, corrosive hydrogen halide gas is not released basically, and the method does not cause damage to operators and operating equipment; and the polybrominated styrene product has excellent color and high whiteness, and the lighter the color is, the wider the application range is as an additive. But the process has long production flow, high requirement on equipment, low bromine content of the product and poor flame retardant effect, so that the product cost is increased, the production period is long, and the market competitiveness of the product is reduced. Chinese patent publication No. CN109867739A discloses a process route of polymerization followed by bromination, which has the advantages of simple process and high bromine content in the product, but the process can cause the main chain to easily undergo bromination reaction, which leads to poor chromaticity and stability of the product and limited application of the product. In China, brominated polystyrene starts late, technical reserve is limited, and the produced brominated polystyrene adopts a process route of firstly polymerizing and then brominating, so that the whiteness and the thermal stability of the product are lower than those of products at foreign countries, and the popularization of the brominated polystyrene in China is seriously influenced.
In order to solve the problems of low whiteness and poor thermal stability of domestic brominated polystyrene, a Chinese patent document with an authorization publication number of CN100540572C proposes that metallic sodium or metallic hydride is used as a reducing agent, a product is dissolved in tetrahydrofuran, heated and refluxed, and then evaporated, crystallized and filtered to obtain a product with good thermal stability and high melt index, but the method has large consumption of the metal or the metallic hydride, and the reaction condition of the method is harsh, sensitive to water, high in cost and not beneficial to industrial production.
Disclosure of Invention
The invention aims to solve the problems of poor thermal stability, low whiteness and the like of domestic brominated polystyrene products and provides a post-treatment method of brominated polystyrene so as to solve the problems. The invention removes bromine on the main chain of the brominated polystyrene by carrying out selective hydrogenation reaction on the brominated polystyrene product, thereby improving the thermal stability and whiteness of the product.
The technical scheme of the invention is as follows: a post-treatment method of brominated polystyrene comprises the following specific steps:
preparing a brominated polystyrene crude product into a solution in a reaction kettle by using a solvent, adding raney nickel and an alkali source into the solution, replacing air in the kettle by using hydrogen, continuously adding the hydrogen, regulating the pressure to 0.1-1MPa, and preserving the heat at the temperature of 25-50 ℃ for 0.5-5h; after the heat preservation is finished, washing the reaction finished liquid with water until the water phase is neutral, taking the organic phase, dropwise adding the organic phase into boiling water for evaporation crystallization, and filtering and drying to obtain a brominated polystyrene finished product.
The bromine content of the brominated polystyrene crude product is 69.1-69.8%, the 1% thermal weight loss temperature is 320-330 ℃, the 5% thermal weight loss temperature is 350-360 ℃, and the whiteness is 50-55%.
The solvent is one of tetrahydrofuran, 1, 4-dioxane, toluene, dichloromethane and 1, 2-dichloroethane; the mass ratio of the brominated polystyrene crude product to the solvent is 5-20.
The mass ratio of the Raney nickel to the brominated polystyrene crude product is 0.1-1.
The alkali source is one of triethylamine, pyridine, sodium hydroxide, sodium carbonate, sodium bicarbonate and sodium tert-butoxide; the mass ratio of the alkali source to the crude brominated polystyrene product is 1-20.
Has the advantages that:
the invention has the advantages that the whiteness and the thermal stability of the product are obviously improved by carrying out the hydrotreatment on the brominated polystyrene, the bromine content of the product is not obviously reduced, the invention has certain selectivity, and the bromine on the benzene ring of the brominated polystyrene can not be removed.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, shall fall within the protection scope of the present invention.
Example 1
The raw material used in this example was a commercially available brominated polystyrene crude product having a bromine content of 69.1%, a 1% thermogravimetric temperature of 330 ℃, a 5% thermogravimetric temperature of 360 ℃, and a whiteness of 55%.
A1L reactor was charged with 20g of crude brominated polystyrene, 0.2g of Raney nickel, 0.2g of triethylamine and 400g of 1, 2-dichloroethane. And (3) replacing 3 times by hydrogen to remove air after the kettle is sealed and pressure tested to be qualified, then introducing hydrogen to regulate the pressure to 1MPa, heating to 25 ℃, and preserving heat for 5 hours. And after the heat preservation is finished, washing the reaction finished liquid by using water, then separating out an organic phase, washing the organic phase by using water until the water phase is neutral, dripping the separated organic phase into boiling water after the washing is finished, evaporating and crystallizing, and filtering and drying to obtain 19.2g of a brominated polystyrene finished product. The whiteness of the product was 86%, the bromine content was 67.4%, the 1% thermal weight loss Temperature (TGA) was 354 ℃, and the 5% TGA was 381 ℃.
Example 2
The raw material used in this example was a commercially available crude brominated polystyrene product having a bromine content of 69.1%, a 1% thermogravimetric loss temperature of 330 ℃, a 5% thermogravimetric loss temperature of 360 ℃ and a whiteness of 55%.
A1L reactor was charged with 20g of crude brominated polystyrene, 0.02g of Raney nickel, 2g of pyridine and 100g of tetrahydrofuran. After the pressure test is qualified, the air is removed by replacing 3 times with hydrogen, then hydrogen is introduced to regulate the pressure to 0.5MPa, the temperature is raised to 50 ℃, and the temperature is kept for 0.5h. And after the heat preservation is finished, washing the reaction finished liquid with water, then separating out an organic phase, washing the organic phase with water until the water phase is neutral, dripping the separated organic phase into boiling water after the washing is finished, evaporating and crystallizing, and filtering and drying to obtain 19.1g of brominated polystyrene finished product. The whiteness of the product was 82%, the bromine content was 67.2%,1% TGA was 356 ℃ and 5% TGA was 383 ℃.
Example 3
The raw material used in this example was an untreated crude brominated polystyrene product having a bromine content of 69.8%, a 1% thermogravimetric temperature of 320 ℃, a 5% thermogravimetric temperature of 350 ℃ and a whiteness of 50%.
A1L reactor was charged with 20g of crude brominated polystyrene, 0.05g of Raney nickel, 0.4g of sodium hydroxide, and 200g of methylene chloride. After the pressure test is qualified, replacing 3 times with hydrogen to remove air, then introducing hydrogen to regulate the pressure to 1MPa, heating to 30 ℃, and preserving the heat for 1h. And after the heat preservation is finished, washing the reaction finished liquid with water, then separating out an organic phase, washing the organic phase with water until the water phase is neutral, dripping the separated organic phase into boiling water after the washing is finished, evaporating and crystallizing, and filtering and drying to obtain 18.8g of brominated polystyrene finished product. The whiteness of the product was 86%, the bromine content was 67.1%,1% TGA was 355 ℃ and 5% TGA was 383 ℃.
Example 4
The raw material used in this example was an untreated crude brominated polystyrene product having a bromine content of 69.8%, a 1% thermogravimetric loss temperature of 320 ℃, a 5% thermogravimetric loss temperature of 350 ℃, and a whiteness of 50%.
A1L reactor was charged with 20g of crude brominated polystyrene, 0.05g of Raney nickel, 1g of sodium carbonate and 200g of toluene. And (3) replacing 3 times with hydrogen to remove air after the pressure test of the closed kettle is qualified, then introducing hydrogen to regulate the pressure to 0.2MPa, heating to 30 ℃, and preserving heat for 2 hours. And after the heat preservation is finished, washing the reaction finished liquid by using water, then separating out an organic phase, washing the organic phase by using water until the water phase is neutral, dripping the separated organic phase into boiling water after the washing is finished, evaporating and crystallizing, and filtering and drying to obtain 19.2g of a brominated polystyrene finished product. The product whiteness is 83%, the bromine content is 68.1%,1% by weight of the TGA is 350 ℃,5% by weight of the TGA is 376 ℃.
Example 5
The raw material used in this example was an untreated crude brominated polystyrene product having a bromine content of 69.4%, a 1% thermogravimetric loss temperature of 324 ℃, a 5% thermogravimetric loss temperature of 356 ℃, and a whiteness of 52%.
20g of crude brominated polystyrene, 0.1g of Raney nickel, 1g of sodium tert-butoxide and 200g of 1, 4-dioxane were added into a 1L reaction kettle. And (3) replacing 3 times with hydrogen to remove air after the pressure test of the closed kettle is qualified, then introducing hydrogen to regulate the pressure to 0.2MPa, heating to 40 ℃, and preserving heat for 3 hours. And after the heat preservation is finished, washing the reaction finished liquid with water, then separating out an organic phase, washing the organic phase with water until the water phase is neutral, dripping the separated organic phase into boiling water after the washing is finished, evaporating and crystallizing, and filtering and drying to obtain 18.8g of brominated polystyrene finished product. The product whiteness is 88%, the bromine content is 67.6%,1% by TGA is 354 ℃,5% by TGA is 382 ℃.
Example 6
The raw material used in this example was an untreated crude brominated polystyrene product having a bromine content of 69.4%, a 1% thermogravimetric loss temperature of 324 ℃, a 5% thermogravimetric loss temperature of 356 ℃, and a whiteness of 52%.
A1L reactor was charged with 20g of crude brominated polystyrene, 0.1g of Raney nickel, 0.5g of sodium bicarbonate, and 300g of methylene chloride. After the pressure test is qualified, replacing 3 times with hydrogen to remove air, then introducing hydrogen to regulate the pressure to 0.5MPa, heating to 30 ℃, and preserving the heat for 1h. And after the heat preservation is finished, washing the reaction finished liquid with water, then separating out an organic phase, washing the organic phase with water until the water phase is neutral, dripping the separated organic phase into boiling water after the washing is finished, evaporating and crystallizing, and filtering and drying to obtain 19.0g of brominated polystyrene finished product. The product whiteness is 84%, the bromine content is 67.4%,1% by weight of the TGA is 352 ℃,5% by weight of the TGA is 378 ℃.
Example 7
The raw material used in this example was a commercially available crude brominated polystyrene product having a bromine content of 69.1%, a 1% thermogravimetric loss temperature of 330 ℃, a 5% thermogravimetric loss temperature of 360 ℃ and a whiteness of 55%.
A1L reactor was charged with 20g of crude brominated polystyrene, 0.02g of Raney nickel, 4g of pyridine and 100g of tetrahydrofuran. After the pressure test is qualified, the air is removed by replacing 3 times with hydrogen, then hydrogen is introduced to regulate the pressure to 0.1MPa, the temperature is raised to 50 ℃, and the temperature is kept for 0.5h. And after the heat preservation is finished, washing the reaction finished liquid with water, then separating out an organic phase, washing the organic phase with water until the water phase is neutral, dripping the separated organic phase into boiling water after the washing is finished, evaporating and crystallizing, and filtering and drying to obtain 19.1g of brominated polystyrene finished product. The whiteness of the product was 82%, the bromine content was 67.5%,1% TGA was 358 ℃,5% TGA was 384 ℃.
Aging the brominated polystyrene finished product obtained in the above example and the brominated polystyrene crude product used in the above example at 200 ℃, and measuring 1% TGA by using a thermal weight loss instrument; measuring whiteness by a whiteness meter; and (4) measuring the bromine content by adopting a combustion method and a potentiometric titrator.
As can be seen from Table 1, the thermal stability and whiteness of the brominated polystyrene crude product after hydrogenation reduction by the method are obviously improved, and the bromine content is not obviously reduced, which indicates that the hydrogenation reduction reaction has selectivity and can remove bromine on the main chain of the brominated polystyrene crude product without removing bromine on a benzene ring.
In addition to the above embodiments, the present invention also includes other embodiments, and any technical solutions formed by equivalent transformation or equivalent replacement should fall within the scope of the claims of the present invention.
Claims (5)
1. A brominated polystyrene post-treatment method is characterized by comprising the following steps:
preparing a brominated polystyrene crude product into a solution in a reaction kettle by using a solvent, adding raney nickel and an alkali source into the solution, replacing air in the kettle by using hydrogen, continuously adding the hydrogen, regulating the pressure to 0.1-1MPa, and preserving the heat at the temperature of 25-50 ℃ for 0.5-5h; after the heat preservation is finished, washing the reaction finished liquid with water until the water phase is neutral, taking the organic phase, dropwise adding the organic phase into boiling water for evaporation crystallization, and filtering and drying to obtain a brominated polystyrene finished product.
2. The post-treatment method of brominated polystyrene as claimed in claim 1, wherein the bromine content of the crude brominated polystyrene product is 69.1-69.8%, the temperature of 1% thermal weight loss is 320-330 ℃, the temperature of 5% thermal weight loss is 350-360 ℃, and the whiteness is 50-55%.
3. The method of claim 1, wherein the solvent is one of tetrahydrofuran, 1, 4-dioxane, toluene, methylene chloride, and 1, 2-dichloroethane; the mass ratio of the brominated polystyrene crude product to the solvent is 5-20.
4. The method for post-treating brominated polystyrene according to claim 1, wherein the mass ratio of the raney nickel to the crude brominated polystyrene is 0.1-1.
5. The post-treatment method of brominated polystyrene according to claim 1, wherein the alkali source is one of triethylamine, pyridine, sodium hydroxide, sodium carbonate, sodium bicarbonate and sodium tert-butoxide; the mass ratio of the alkali source to the crude brominated polystyrene product is 1-20.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1275992A (en) * | 1997-11-18 | 2000-12-06 | 费罗公司 | Process for the preparation of brominated polystyrene having improved color characteristics |
| US20020035214A1 (en) * | 1996-06-14 | 2002-03-21 | Ferro Corporation | Brominated polystyrene having improved thermal stability and color and process for the preparation thereof |
| CN101085819A (en) * | 2007-05-19 | 2007-12-12 | 芜湖沃特工程技术有限公司 | Preparation method for brominated polystyrene |
| 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 |
| CN109694419A (en) * | 2018-12-27 | 2019-04-30 | 山东旭锐新材有限公司 | BPS product and preparation method thereof by full bromine method |
-
2022
- 2022-12-26 CN CN202211670260.0A patent/CN115636888A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020035214A1 (en) * | 1996-06-14 | 2002-03-21 | Ferro Corporation | Brominated polystyrene having improved thermal stability and color and process for the preparation thereof |
| CN1275992A (en) * | 1997-11-18 | 2000-12-06 | 费罗公司 | Process for the preparation of brominated polystyrene having improved color characteristics |
| CN101085819A (en) * | 2007-05-19 | 2007-12-12 | 芜湖沃特工程技术有限公司 | Preparation method for brominated polystyrene |
| 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 |
| CN109694419A (en) * | 2018-12-27 | 2019-04-30 | 山东旭锐新材有限公司 | BPS product and preparation method thereof by full bromine method |
Non-Patent Citations (1)
| Title |
|---|
| 刘琪等: "Raney Ni催化4-溴联苯加氢降解研究" * |
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Application publication date: 20230124 |