CN103333428B - A kind of preparation method of Zero halogen flame resistance polyethylene waterproof roll - Google Patents
A kind of preparation method of Zero halogen flame resistance polyethylene waterproof roll Download PDFInfo
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- CN103333428B CN103333428B CN201310216781.3A CN201310216781A CN103333428B CN 103333428 B CN103333428 B CN 103333428B CN 201310216781 A CN201310216781 A CN 201310216781A CN 103333428 B CN103333428 B CN 103333428B
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Abstract
The invention discloses a kind of preparation method of Zero halogen flame resistance polyethylene waterproof roll, feature is that this preparation method comprises the steps: to get by weight 100 parts of composite flame-retardant agents, 1-4 part coupling agent diluent to drop in homogenizer at 80 DEG C stir process 30 minutes, obtains modified flame-retardant agent stand-by after drying and grinding; Get polyethylene (PE) by weight and expect that 65-80 part is dropped into homogenizer mix 15 minutes with the modified flame-retardant agent 60-80 part obtained, plasticized modifier 5-25 part, retardant synergist 10-15 part, initiator 0.1-1 part, composite antioxidant 0.3-3 part, catalyzer 0.5-1 part above, for subsequent use with twin screw extruder extruding pelletization; By pellet sulfuration on vulcanizing press, curing time 10min, cold pressing 5min, and the waterproof roll finished product of different size made by the mould finally by different thickness.
Description
Technical field
The present invention relates to a kind of preparation method of Zero halogen flame resistance polyethylene waterproof roll, this waterproof roll is mainly used in building trade aspect.
Background technology
Polyethylene (PE) waterproof roll plays an important role in roof waterproof, but its flame retardant properties is very poor, limiting oxygen index(LOI) (LOI) is only 17.3 and belongs to inflammable material, during burning, a large amount of oxygen consumption releases strong flue gas, be the major reason causing loss of life and personal injury in fire, therefore common PE waterproof roll is more and more difficult to the requirement meeting building roof fire safety.
If inflammable PE waterproof roll is very fast from putting out after not easily being lighted or light, or light afterfire speed very slowly, will greatly reduce the generation of fire, usually will reach this purpose just needs to add fire retardant.The fire retardant of domestic more than 80% is halogenated flame retardant at present, generates more cigarette, corrosive gases and toxic gas, even can produce the carcinogenic substances such as dioxin in some cases during its burning.European Union " forbids Hazardous Substances Directive in electronic and electrical equipment " and sternly states: the halogenated flame retardant that the electric type product throwing in EU market afterwards on July 1st, 2006 must not be harmful to containing Polybrominated biphenyl etc.Based on the understanding to environment protection, the fire-retardant of polymer materials has tended to non-halogen conversion.
But due to incendivity and the fire retardant mechanism of PE, the flame retarding efficiency of halogen-free flame retardants is difficult to the degree reaching some Halogen flame-retardant systems, thus causes the increase of amount of flame-retardant agent, and the mechanical property of waterproof roll also decreases.Therefore, how improved the flame retarding efficiency of waterproof roll by halogen-free flame retardants, can improve again its mechanical property becomes problem demanding prompt solution simultaneously.
Summary of the invention
The object of the invention is for overcoming the deficiencies in the prior art, the preparation method of the polyethylene waterproof roll of a kind of Halogen, efficient, good mechanical properties is provided.
To achieve these goals, the preparation method of Zero halogen flame resistance polyethylene waterproof roll of the present invention intends by the following technical solutions: adopt twin screw extruder, mill, vulcanizing press as reactor, using modified magnesium hydroxide, modified aluminium hydroxide, modification magnesium aluminum-hydrotalcite, microcapsule red phosphorus, ammonium polyphosphate modifying as composite halogen-free flame retardants, styrene-maleic anhydride copolymer (SMA) as retardant synergist, prepares novel flame-proof polyethylene waterproof roll as plasticized modifier, silicon rubber.And the indexs such as the oxygen index of test system, vertical combustion grade, tensile strength and elongation at break.
The preparation method of Zero halogen flame resistance polyethylene waterproof roll of the present invention comprises the steps:
1) step one: the modification of fire retardant: get 60-80 part composite flame-retardant agent by weight, 1-4 part coupling agent diluent to drop in homogenizer at temperature condition is 80 DEG C stir process 30 minutes, obtain modified flame-retardant agent after drying and grinding stand-by;
2) step 2: get modified flame-retardant agent 60-80 part that polyethylene (PE) expects that 65-80 part and step one obtain by weight, plasticized modifier 5-25 part, retardant synergist 10-15 part, initiator 0.1-1 part, composite antioxidant 0.3-3 part, catalyzer 0.5-1 part drops into homogenizer and mix 15 minutes, then use twin screw extruder extruding pelletization for subsequent use;
3) step 3: pellet step 2 obtained first opens sulfuration on vulcanizing press again after refining by mill, and curing time 10min, cold pressing 5min, and the waterproof roll finished product of different size made by the mould finally by different thickness.
Further, aforesaid composite flame-retardant agent can be that modified magnesium hydroxide, modified aluminium hydroxide and microcapsule red phosphorus are composite; Aforesaid composite flame-retardant agent also can be that modified magnesium hydroxide, modified aluminium hydroxide and ammonium polyphosphate modifying (APP) are composite; Aforesaid composite flame-retardant agent also can be that modification magnesium aluminum-hydrotalcite and microcapsule red phosphorus are composite; Aforesaid composite flame-retardant agent can also be that modification magnesium aluminum-hydrotalcite and modification APP are composite.
Further, aforesaid plasticized modifier can be styrene-maleic anhydride copolymer (SMA).
Further, aforesaid retardant synergist is silicon rubber.
Further, aforesaid coupling agent diluent, after being mixed with titanic acid ester by silane coupling agent, is mixed with using white oil as thinner.
Further, aforesaid silane coupling agent can be one in vinyltrimethoxy silane (A-171) or vinyl three ('beta '-methoxy oxyethyl group) silane (A-172) or combination.
Further, aforesaid antioxidant is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, thio-2 acid octadecyl ten diester, the composite use of N, N'-bis-salicylidene propylene diamine.
Further, aforesaid initiator is dicumyl peroxide (DCP), and aforesaid catalyzer is dibutyl tin laurate.
Further, in step 2, the temperature control of twin screw extruder is: 130-260 DEG C; Step 3 middle plateform vulcanizer mold temperature is 180 DEG C, pressure 15MPa.
In addition, also can add smoke suppressant during preparation or press down dripping agent to improve the flame retardant properties of product.Anti UV agent also can be added to improve the ageing resistance of product during preparation.Lubricant or releasing agent also can be added to improve the processing characteristics of product during preparation.
Compared with the prior art, owing to have employed technical scheme of the present invention, the Zero halogen flame resistance polyethylene waterproof roll tensile strength prepared according to preparation method of the present invention can reach 16-19MPa, elongation at break can reach 200-400%, oxygen index can reach 25-29%, vertical combustion grade can reach FV-0-FV-1 level, and impervious index can reach: 30min, 0.3MPa do not seep water.The Zero halogen flame resistance polyethylene waterproof roll prepared according to preparation method of the present invention can be used for construction waterproofing engineering, has broad application prospects.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
(1) preparation of silane coupling agent: by weight the mixed solution of 15 parts of vinyltrimethoxy silanes (A-171) and 10 parts of titanic acid ester is mixed with white oil 80 parts, be mixed with coupling agent diluent;
(2) step one: the modification of fire retardant: get magnesium hydroxide 50 parts, 10 parts, aluminium hydroxide silane coupling agent and titanic acid ester mixed diluting liquid 2 parts by weight and process 30 minutes at 80 DEG C of temperature in homogenizer, obtain modified flame-retardant agent after drying and grinding stand-by;
(3) step 2: get polyethylene (PE) by weight and expect 80 parts, step one the modification compound flame retardant 60 parts, microcapsule red phosphorus 15 parts, plasticized modifier styrene-maleic anhydride copolymer (SMA) 15 parts, 10 parts, silicon rubber, initiator DCP 0.5 part, composite antioxidant 1 part, the catalyst dibutyltin dilaurylate 1 part that obtain, 15 minutes are mixed by homogenizer, for subsequent use with twin screw extruder extruding pelletization;
(4) step 3: pellet step 2 obtained first opens sulfuration on vulcanizing press again after refining by mill, and curing time 10min, cold pressing 5min, and the waterproof roll finished product of different size made by the mould finally by different thickness.
Embodiment 2
(1) preparation of silane coupling agent: by weight the mixed solution of 15 parts of A-172 and 10 part titanic acid ester and white oil 80 parts is mixed, be mixed with coupling agent diluent;
(2) step one: the modification of fire retardant: get magnesium hydroxide 50 parts by weight, 10 parts, aluminium hydroxide is re-dubbed composite flame-retardant agent with APP15 part, and at homogenizer 80 DEG C of temperature, process 30 minutes with silane coupling agent and titanic acid ester mixed diluting liquid 3 parts, obtain modified flame-retardant agent after drying and grinding stand-by;
(3) step 2: get polyethylene (PE) by weight and expect 80 parts, step one the modification compound flame retardant 75, plasticized modifier styrene-maleic anhydride copolymer (SMA) 15 parts, 10 parts, silicon rubber, initiator DCP 0.5 part, composite antioxidant 1 part, the catalyst dibutyltin dilaurylate 1 part that obtain, 15 minutes are mixed by homogenizer, for subsequent use with twin screw extruder extruding pelletization;
(4) step 3: pellet step 2 obtained first opens sulfuration on vulcanizing press again after refining by mill, and curing time 10min, cold pressing 5min, and the waterproof roll finished product of different size made by the mould finally by different thickness.
Embodiment 3
(1) preparation of silane coupling agent: by weight the mixed solution of 15 parts of A-171 and 10 part titanic acid ester and white oil 80 parts is mixed, be mixed with coupling agent diluent;
(2) step one: the modification of fire retardant: get magnesium aluminum-hydrotalcite 60 parts by weight, and at homogenizer 80 DEG C of temperature, process 30 minutes with silane coupling agent and titanic acid ester mixed diluting liquid 2 parts, obtain modified flame-retardant agent after drying and grinding stand-by;
(3) step 2: get polyethylene (PE) by weight and expect 80 parts, step one the modification magnesium aluminum-hydrotalcite 60 parts, microcapsule red phosphorus 15 parts, plasticized modifier styrene-maleic anhydride copolymer (SMA) 15 parts, 10 parts, silicon rubber, initiator DCP 0.5 part, composite antioxidant 1 part, the catalyst dibutyltin dilaurylate 1 part that obtain, 15 minutes are mixed by homogenizer, for subsequent use with twin screw extruder extruding pelletization;
(4) step 3: pellet step 2 obtained first opens sulfuration on vulcanizing press again after refining by mill, and curing time 10min, cold pressing 5min, and the waterproof roll finished product of different size made by the mould finally by different thickness.
Embodiment 4
(1) preparation of silane coupling agent: by weight the mixed solution of 15 parts of A-171 and 10 part titanic acid ester and white oil 80 parts is mixed, be mixed with coupling agent diluent;
(2) step one: the modification of fire retardant: get magnesium aluminum-hydrotalcite 60 parts by weight, APP15 part also processes 30 minutes with silane coupling agent and titanic acid ester mixed diluting liquid 3 parts at homogenizer 80 DEG C of temperature, obtain modified flame-retardant agent after drying and grinding stand-by;
(3) step 2: get polyethylene (PE) by weight and expect 80 parts, step one the modification compound flame retardant 75 parts, plasticized modifier styrene-maleic anhydride copolymer (SMA) 15 parts, 10 parts, silicon rubber, initiator DCP 0.5 part, composite antioxidant 1 part, the catalyst dibutyltin dilaurylate 1 part that obtain, 15 minutes are mixed by homogenizer, for subsequent use with twin screw extruder extruding pelletization;
(4) step 3: pellet step 2 obtained first opens sulfuration on vulcanizing press again after refining by mill, and curing time 10min, cold pressing 5min, made the waterproof roll finished product of different size by the mould of different thickness.
Certainly, the embody rule example of more than just invention, the technical scheme that the present invention also has other embodiment, all employings to be equal to replacement or equivalent transformation to be formed, all drops within protection domain of the presently claimed invention.
Claims (7)
1. a preparation method for Zero halogen flame resistance polyethylene waterproof roll, is characterized in that this preparation method comprises the steps:
1) step one: the modification of fire retardant: get 60-80 part composite flame-retardant agent by weight, 1-4 part coupling agent diluent to drop in homogenizer at temperature condition is 80 DEG C stir process 30 minutes, obtain modified flame-retardant agent after drying and grinding stand-by;
2) step 2: get modified flame-retardant agent 60-80 part that polyethylene (PE) expects that 65-80 part and step one obtain by weight, plasticized modifier 5-25 part, retardant synergist 10-15 part, initiator 0.1-1 part, composite antioxidant 0.3-3 part, catalyzer 0.5-1 part drops into homogenizer and mix 15 minutes, then use twin screw extruder extruding pelletization for subsequent use;
3) step 3: pellet step 2 obtained first opens sulfuration on vulcanizing press again after refining by mill, curing time 10min, and cold pressing 5min, and the waterproof roll finished product of different size made by the mould finally by different thickness;
Described composite flame-retardant agent be modification magnesium aluminum-hydrotalcite and microcapsule red phosphorus is composite or modification magnesium aluminum-hydrotalcite and modification APP composite.
2. the preparation method of Zero halogen flame resistance polyethylene waterproof roll according to claim 1, is characterized in that: described plasticized modifier is styrene-maleic anhydride copolymer (SMA).
3. the preparation method of Zero halogen flame resistance polyethylene waterproof roll according to claim 1, is characterized in that: described retardant synergist: silicon rubber, and alternative part polyethylene increases Flame Retardancy energy.
4. the preparation method of Zero halogen flame resistance polyethylene waterproof roll according to claim 1, is characterized in that: described coupling agent diluent, after being mixed by a certain percentage with titanic acid ester by silane coupling agent, is mixed with using white oil as thinner.
5. the preparation method of Zero halogen flame resistance polyethylene waterproof roll according to claim 4, is characterized in that: described silane coupling agent is one in vinyltrimethoxy silane (A-171) or vinyl three ('beta '-methoxy oxyethyl group) silane (A-172) or combination.
6. the preparation method of Zero halogen flame resistance polyethylene waterproof roll according to claim 1, it is characterized in that: described composite antioxidant is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, thio-2 acid octadecyl ten diester, the composite use of N, N'-bis-salicylidene propylene diamine.
7. the preparation method of Zero halogen flame resistance polyethylene waterproof roll according to claim 1, is characterized in that: described initiator is dicumyl peroxide (DCP), and described catalyzer is dibutyl tin laurate.
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| CN105440564B (en) * | 2015-12-30 | 2018-06-29 | 衢州学院 | A kind of halogen-free flame-retardant ABS composite material and preparation method thereof |
| CN106366398A (en) * | 2016-08-27 | 2017-02-01 | 潍坊市宏源防水材料有限公司 | Peroxide cross-linked polyolefin waterproof coiled material and preparation technology thereof |
| CN109486124A (en) * | 2018-10-10 | 2019-03-19 | 深圳市富恒新材料股份有限公司 | A kind of halogen-free flame-retardant glass fiber enhancing PBT material and preparation method thereof |
| CN110128966A (en) * | 2019-06-10 | 2019-08-16 | 山东省金帅防水材料有限公司 | A kind of halogen-free flame-retardant waterproof roll and preparation method thereof and preparation method thereof |
| CN112159560A (en) * | 2020-09-27 | 2021-01-01 | 威海联桥新材料科技股份有限公司 | Silicone rubber-silane crosslinked polyethylene blending material and preparation method thereof |
| CN115433399B (en) * | 2022-10-09 | 2024-01-30 | 廊坊北化高分子材料有限公司 | Flame-retardant waterproof thermoplastic elastomer material, preparation method and waterproof coiled material |
| CN115926288A (en) * | 2022-12-08 | 2023-04-07 | 合肥兴联通讯有限公司 | Elastomer toughened and crosslinked HDPE halogen-free smoke-suppression flame-retardant cable material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276899A (en) * | 2011-07-18 | 2011-12-14 | 武汉钢铁(集团)公司 | Magnesium hydroxide flame-retardant composite material and preparation method thereof |
| CN102464833A (en) * | 2010-11-08 | 2012-05-23 | 天津市耀新科技发展有限公司 | Waterproof flame-retarding composite coiled material and preparation method thereof |
| CN102898722A (en) * | 2011-07-24 | 2013-01-30 | 天津市耀新科技发展有限公司 | Modified polypropylene waterproof coiled material and preparation method thereof |
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| JPH0562521A (en) * | 1991-09-04 | 1993-03-12 | Hitachi Cable Ltd | Polyolefin insulating material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464833A (en) * | 2010-11-08 | 2012-05-23 | 天津市耀新科技发展有限公司 | Waterproof flame-retarding composite coiled material and preparation method thereof |
| CN102276899A (en) * | 2011-07-18 | 2011-12-14 | 武汉钢铁(集团)公司 | Magnesium hydroxide flame-retardant composite material and preparation method thereof |
| CN102898722A (en) * | 2011-07-24 | 2013-01-30 | 天津市耀新科技发展有限公司 | Modified polypropylene waterproof coiled material and preparation method thereof |
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