CN112876780A - Environment-friendly flame-retardant expandable polystyrene resin and preparation method thereof - Google Patents
Environment-friendly flame-retardant expandable polystyrene resin and preparation method thereof Download PDFInfo
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- CN112876780A CN112876780A CN202110020360.8A CN202110020360A CN112876780A CN 112876780 A CN112876780 A CN 112876780A CN 202110020360 A CN202110020360 A CN 202110020360A CN 112876780 A CN112876780 A CN 112876780A
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- 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 title claims abstract description 31
- 239000003063 flame retardant Substances 0.000 title claims abstract description 31
- 229920006248 expandable polystyrene Polymers 0.000 title claims abstract description 19
- 229920005989 resin Polymers 0.000 title claims abstract description 16
- 239000011347 resin Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 32
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical class C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 12
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 12
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 12
- 239000004698 Polyethylene Substances 0.000 claims description 10
- -1 polyethylene Polymers 0.000 claims description 10
- 229920000573 polyethylene Polymers 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 7
- 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 claims description 7
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 7
- 239000001506 calcium phosphate Substances 0.000 claims description 7
- 235000011010 calcium phosphates Nutrition 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 7
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000003607 modifier Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000009413 insulation Methods 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- DEIGXXQKDWULML-UHFFFAOYSA-N 1,2,5,6,9,10-hexabromocyclododecane Chemical compound BrC1CCC(Br)C(Br)CCC(Br)C(Br)CCC1Br DEIGXXQKDWULML-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000010557 suspension polymerization reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/16—Making expandable particles
- C08J9/18—Making expandable particles by impregnating polymer particles with the blowing agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0033—Use of organic additives containing sulfur
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/141—Hydrocarbons
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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Abstract
The invention relates to an environment-friendly flame-retardant expandable polystyrene resin and a preparation method thereof. The sectional polymerization technology adopted by the new process can effectively solve the problem of the compatibility of the brominated styrene-butadiene-styrene block copolymer and styrene, and effectively improve the flame retardant efficiency. The environment-friendly flame-retardant expandable polystyrene resin prepared by the invention has ecological environment protection and biological safety, can meet the requirements of European and American places and the like for ground outlet, has flame retardance meeting the requirements of the field of building exterior wall heat insulation, and has wide application prospect.
Description
Technical Field
The invention relates to the field of polystyrene resin, in particular to environment-friendly flame-retardant expandable polystyrene resin and a preparation method thereof.
Background
At present, although the flame retardant used in the market has the advantage of high cost performance, the flame retardant cannot be used for export because the flame retardant cannot meet the stockholm convention. The substitute flame retardant mainly comprises methyl octabromoether and brominated styrene-butadiene-styrene block copolymer, wherein the methyl octabromoether is not listed as an illegal substance, but the brominated styrene-butadiene-styrene block copolymer has more ecological environmental protection and biological safety in the long term, so the brominated styrene-butadiene-styrene block copolymer is preferably used as the novel flame retardant. However, when the copolymer is used for suspension polymerization in a reactor, the copolymer has the problem of compatibility with styrene, so that the flame retardant can only be increased to achieve the same flame retardant effect as hexabromocyclododecane, and the flame retardant effect is influenced to a certain extent if the flame retardant is excessively added, so that the cost is increased and the production efficiency is reduced.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide an environment-friendly flame-retardant expandable polystyrene resin which adopts brominated styrene-butadiene-styrene block copolymer as a novel flame retardant and is compatible with styrene during suspension polymerization in a reactor so as to meet the requirements of ecological environment protection and biological safety, and the technical purpose is realized by the following technical scheme:
the environment-friendly flame-retardant expandable polystyrene resin is prepared from the following raw materials in parts by weight: 90-110 parts of styrene; 100-130 parts of desalted water; 0.0002 to 0.0005 part of sodium sulfonate; 1.2-4.0 parts of calcium phosphate; 0.3-0.5 parts of benzoyl peroxide; 0.3-0.6 part of dicumyl peroxide; 0.75-0.9 part of brominated styrene-butadiene-styrene block copolymer; 4.0-5.0 parts of pentane; 0.1-0.3 part of structure regulator.
Preferably: the structure modifier is linear polyethylene or branched polyethylene.
The invention also provides a preparation method of the environment-friendly flame-retardant expandable polystyrene resin, which comprises the following steps:
s1: introducing desalted water into a reactor, uniformly stirring, sequentially adding calcium phosphate and sodium sulfonate, continuously stirring for 5-10 minutes, and then sequentially adding half of styrene and half of benzoyl peroxide;
s2: heating the reactor, then entering a constant temperature stage, and preserving heat;
s3: adding the rest styrene and benzoyl peroxide, dicumyl peroxide, brominated styrene-butadiene-styrene block copolymer and a structure regulator, continuing to heat, entering a constant temperature two stage, and preserving heat to enable the materials to form particles;
s4: adding pentane, continuously heating, setting the temperature and pressure of the reaction, and keeping the temperature and pressure until the reaction is finished;
s5: and (3) reducing the temperature of the materials in the reactor to below 50 ℃, and dehydrating to obtain the environment-friendly flame-retardant expandable polystyrene resin.
The specific process parameters are as follows:
in the step S2, the temperature rising speed is 0.6-1.2 ℃/min, the temperature in the constant temperature stage is 85-93 ℃, and the heat preservation holding time is 100-150 min.
In the step S3, the temperature of the constant temperature stage is 85-90 ℃, and the heat preservation time is 300-360 minutes.
In the step S4, the reaction temperature is 110-130 ℃, the pressure is 0.8-1.0 Mpa, and the reaction time is 240-300 minutes.
The invention has the beneficial effects that: the sectional polymerization technology adopted by the invention effectively solves the problem of compatibility of the brominated styrene-butadiene-styrene block copolymer and styrene, and improves the flame retardant efficiency. The flame retardant is non-hexabromoflame retardant EPS, has ecological environmental protection and biological safety, can meet the requirements of Europe and America and the like on ground outlet, has flame retardance meeting the requirements of the field of building external wall heat insulation, and has wide application prospect.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention.
Detailed Description
The specific technical scheme of the invention is illustrated by combining the embodiment, and the flow of the invention is shown in figure 1.
Example 1
115 parts of desalted water are poured into the reactor, 2.6 parts of calcium phosphate and 0.0003 part of sodium sulfonate are added in turn with uniform stirring, and stirring is continued for 8 minutes. 50 parts of styrene and 0.2 part of benzoyl peroxide are added in sequence, the reactor is heated at a heating rate of 0.9 ℃/minute, and when the temperature rises to 89 ℃, the temperature is kept constant for 125 minutes.
The remaining 50 parts of styrene, the remaining 0.2 part of benzoyl peroxide, 0.5 part of dicumyl peroxide, 0.8 part of brominated styrene-butadiene-styrene block copolymer and 0.2 part of a structure modifier, which is linear polyethylene or branched polyethylene, are added and the reactor is further warmed. When the temperature was raised to 88 ℃, the material was granulated by holding the temperature constant for 330 minutes.
4.5 parts of pentane are added and the reactor is heated further to a temperature of 120 ℃ to a pressure of 0.9MPa and maintained at this pressure for 270 minutes.
And cooling the reactor to reduce the temperature of the materials in the reactor to below 50 ℃.
And finally, dehydrating the material to obtain the expandable polystyrene particles.
Example 2
130 parts of desalted water is poured into a reactor, 4.0 parts of calcium phosphate and 0.0005 part of sodium sulfonate are added in sequence under uniform stirring, and stirring is continued for 10 minutes. Thereafter, 55 parts of styrene and 0.25 part of benzoyl peroxide were added in this order, and the reactor was heated at a rate of 1.2 ℃ per minute, and when the temperature was raised to 93 ℃, the temperature was maintained at a constant temperature for 150 minutes.
The remaining 55 parts of styrene, the remaining 0.25 part of benzoyl peroxide, 0.6 part of dicumyl peroxide, 0.9 part of brominated styrene-butadiene-styrene block copolymer and 0.3 part of a structure modifier, which is linear polyethylene or branched polyethylene, are added and the reactor is further warmed. When the temperature is raised to 90 ℃, the constant temperature is kept for 300 minutes, so that the materials are formed into particles.
4.0 parts of pentane are added and the reactor is heated further to a temperature of 130 ℃ to a pressure of 1.0MPa and held at this pressure for 300 minutes.
And cooling the reactor to reduce the temperature of the materials in the reactor to below 50 ℃.
And finally, dehydrating the material to obtain the expandable polystyrene particles.
Example 3
100 parts of desalted water is poured into the reactor, 1.2 parts of calcium phosphate and 0.0002 part of sodium sulfonate are added in turn with uniform stirring, and stirring is continued for 5 minutes. Thereafter, 45 parts of styrene and 0.15 part of benzoyl peroxide were added in this order, and the reactor was heated at a rate of 0.6 ℃ per minute, and when the temperature was raised to 85 ℃, the temperature was maintained at constant temperature for 100 minutes.
The remaining 45 parts of styrene, the remaining 0.15 parts of benzoyl peroxide, 0.3 part of dicumyl peroxide, 0.75 part of brominated styrene-butadiene-styrene block copolymer and 0.1 part of a structure modifier, wherein the modifier is linear polyethylene or branched polyethylene, are added and the reactor is further heated. When the temperature rises to 85 ℃, the material is kept for 360 minutes at constant temperature to form particles.
5.0 parts of pentane are added and the reactor is heated further to a temperature of 110 ℃ to a pressure of 0.8MPa and held at this pressure for 240 minutes.
And cooling the reactor to reduce the temperature of the materials in the reactor to below 50 ℃.
And finally, dehydrating the material to obtain the expandable polystyrene particles.
The final conversion rate of the product can reach 99.5 to 99.9 percent. The oxygen index of the non-hexabromoEPS product can reach 33.3% (GB/T2406.1-2008& BG/T2406.2-2009) through detection of a relevant mechanism, the horizontal combustion grade HB (GB/T2408 + 2008) and the combustion performance reach the flame-retardant B1(B-s2, d0, T1) grade (GB 2-2012). The test proves that the product can achieve the flame retardant effect of the original hexabromocyclododecane.
Claims (6)
1. An environment-friendly flame-retardant expandable polystyrene resin is characterized in that: the feed is prepared from the following raw materials in parts by weight:
90-110 parts of styrene; 100-130 parts of desalted water; 0.0002 to 0.0005 part of sodium sulfonate; 1.2-4.0 parts of calcium phosphate; 0.3-0.5 parts of benzoyl peroxide; 0.3-0.6 part of dicumyl peroxide; 0.75-0.9 part of brominated styrene-butadiene-styrene block copolymer; 4.0-5.0 parts of pentane; 0.1-0.3 part of structure regulator.
2. The environment-friendly flame-retardant expandable polystyrene resin according to claim 1, wherein: the structure modifier is linear polyethylene or branched polyethylene.
3. The preparation method of the environment-friendly flame retardant expandable polystyrene resin according to claim 1 or 2, wherein: the method comprises the following steps:
s1: introducing desalted water into a reactor, uniformly stirring, sequentially adding calcium phosphate and sodium sulfonate, continuously stirring for 5-10 minutes, and then sequentially adding half of styrene and half of benzoyl peroxide;
s2: heating the reactor, then entering a constant temperature stage, and preserving heat;
s3: adding the rest styrene and benzoyl peroxide, dicumyl peroxide, brominated styrene-butadiene-styrene block copolymer and a structure regulator, continuing to heat, entering a constant temperature two stage, and preserving heat to enable the materials to form particles;
s4: adding pentane, continuously heating, setting the temperature and pressure of the reaction, and keeping the temperature and pressure until the reaction is finished;
s5: and (3) reducing the temperature of the materials in the reactor to below 50 ℃, and dehydrating to obtain the environment-friendly flame-retardant expandable polystyrene resin.
4. The preparation method of the environment-friendly flame retardant expandable polystyrene resin according to claim 3, wherein: in the step S2, the temperature rising speed is 0.6-1.2 ℃/min, the temperature in the constant temperature stage is 85-93 ℃, and the heat preservation time is 100-150 min.
5. The preparation method of the environment-friendly flame retardant expandable polystyrene resin according to claim 3, wherein: in the step S3, the temperature of the constant temperature stage is 85-90 ℃, and the heat preservation time is 300-360 minutes.
6. The preparation method of the environment-friendly flame retardant expandable polystyrene resin according to claim 3, wherein: in the step S4, the reaction temperature is 110-130 ℃, the pressure is 0.8-1.0 Mpa, and the reaction time is 240-300 minutes.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092462A (en) * | 2007-06-14 | 2007-12-26 | 华若中 | Expandable granules of polystyrene and prepartion method |
| CN104194031A (en) * | 2014-08-26 | 2014-12-10 | 北京工商大学 | Preparation method of flame-retardant-containing expandable polystyrene granules |
| CN105175917A (en) * | 2015-09-02 | 2015-12-23 | 天津斯坦利新型材料有限公司 | Flame-resistant expandable styrene polymer composition and manufacturing method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092462A (en) * | 2007-06-14 | 2007-12-26 | 华若中 | Expandable granules of polystyrene and prepartion method |
| CN104194031A (en) * | 2014-08-26 | 2014-12-10 | 北京工商大学 | Preparation method of flame-retardant-containing expandable polystyrene granules |
| CN105175917A (en) * | 2015-09-02 | 2015-12-23 | 天津斯坦利新型材料有限公司 | Flame-resistant expandable styrene polymer composition and manufacturing method thereof |
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