CN103159897A - Method for preparing HMSPP (High Melt Strength Polypropylene) from cross-linked and modified T30s - Google Patents

Method for preparing HMSPP (High Melt Strength Polypropylene) from cross-linked and modified T30s Download PDF

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Publication number
CN103159897A
CN103159897A CN2013100980274A CN201310098027A CN103159897A CN 103159897 A CN103159897 A CN 103159897A CN 2013100980274 A CN2013100980274 A CN 2013100980274A CN 201310098027 A CN201310098027 A CN 201310098027A CN 103159897 A CN103159897 A CN 103159897A
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China
Prior art keywords
hmspp
benzoyl
cross
acetone
peroxidation
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CN2013100980274A
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Chinese (zh)
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杨金明
王波
田小艳
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SHAANXI PROVINCE LIGHT INDUSTRY RESEARCH DESIGN INSTITUTE
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SHAANXI PROVINCE LIGHT INDUSTRY RESEARCH DESIGN INSTITUTE
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Priority to CN2013100980274A priority Critical patent/CN103159897A/en
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Abstract

The method discloses a method for preparing HMSPP (High Melt Strength Polypropylene) through cross-linking and modification of T30s, wherein with 2,5-dimethyl-2,5-bi(tertbutyl peroxo) hexane and peroxide (bi) benzoyl as initiators and dibutyltin dilaurate as a catalyst, vinyl long-chain unsaturated silane is catalyzed to be grafted with cross-linked and modified T30s so as to prepare 20 cN high melt strength polypropylene. The method provided by the invention is even and stable in reaction and the prepared product is high in quality and good in stability,; and the method is economic, low in energy consumption, high in yield, high in melt strength and free from extraneous odor.

Description

Cross-linking modified T30s prepares the method for HMSPP
[technical field]
The invention belongs to polypropylene modification PP Pipe Compound production technical field, relate to a kind of method that cross-linking modified T30s prepares HMSPP.
[background technology]
HMSPP is the polypropylene that a kind of resin contains long-chain branch, long-chain branch is initiation grafting in post polymerization, the melt strength of this homopolymer is to have 9 times of similar flow characteristics plain polypropylene homopolymer, in the situation that density and melt flow rate (MFR) are close, the yield strength of HMSPP, modulus in flexure and heat-drawn wire and fusing point are all higher than plain polypropylene.But notched Izod impact strength is lower than plain polypropylene.
The resin dedicated plain polypropylene thermoforming hard problem that solved of HMSPP, can be on the ordinary hot molding device thin-walled pressure vessel of the larger stretch ratio of moulding, processing temperature a wider range, technique is easily grasped, container wall thickness is even.
[summary of the invention]
For above technical problem, the invention provides a kind of method that cross-linking modified T30s prepares HMSPP, have economy, energy consumption is low, productive rate is high, melt strength is high characteristics.
For solving above technical problem, the present invention by the following technical solutions:
A kind of cross-linking modified T30s prepares the method for HMSPP, with 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane and peroxidation (two) benzoyl is as initiator, make catalyzer with dibutyl tin laurate, catalyzed ethylene base long-chain unsaturated silane graft crosslinking modification T30s prepares the 20cN high melt strength, propylene; According to the mass fraction meter, described 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane is 0.5-2 part, described peroxidation (two) benzoyl is 0.5-1 part, described dibutyl tin laurate is 0.1-2 part, and described vinyl long-chain unsaturated silane is 1-5 part, and described T30s is 95-98 part.
As the preferred embodiments of the present invention, at first described peroxidation (two) benzoyl was dissolved in the acetone of 20-100 part before adding;
As the preferred embodiments of the present invention, described vinyl long-chain unsaturated silane and dibutyl tin laurate add after being dissolved in 4-50 part acetone soln again;
compared with prior art, the method that the cross-linking modified T30s of the present invention prepares HMSPP has the following advantages at least: adopt acetone solution vinyl long-chain unsaturated silane, dibutyl tin laurate is made catalyst modification T30s and is prepared high melt strength, propylene, improve degree of crosslinking, solve high temperature and extruded the problem that is accompanied by a large amount of degradeds in crosslinked situation and makes its degradation, thereby make vinyl unsaturated silane graft crosslinking modified polypropene T30s can obtain high performance HMSPP, adopt dimethyl-2, 5-bis(t-butylperoxy) hexane, the compound initiation of peroxidation (two) benzoyl has solved the peroxidation agent initiator system that contains merely phenyl ring, reach product in production process and easily have the excessive problem that is difficult to remove of peculiar smell.
[embodiment]
The technical solution used in the present invention is as follows:
One step of a kind of T30s is extruded the method for the crosslinked 20cN of preparation high melt strength, propylene, and its production stage is:
The first step is opened twin screw extruder, and the polypropylene T30s that 95-98 part is dried is evenly fed by hopper, and screw speed is that 200-400 turns/min, Heating temperature 180-200 ℃.
Second step, with 0.5-2 part 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, 0.5-1 part peroxidation (two) benzoyl (being dissolved in 20-100 part acetone) mix, and are pumped into by volume pump from forcing machine the second heating module;
The 3rd step was that 1-5 part vinyl long-chain unsaturated silane, 0.1-2 part dibutyl tin laurate and 4-50 part acetone dissolve each other with mass ratio, had volume pump to pump into from forcing machine the 3rd heating module; The adjusting screw(rod) rotating speed, feed rate, volume pump liquid flow rate make each raw material simultaneous reactions complete, and the acetone reduction vaporization is reclaimed.Cooling and dicing after melt extrusion.
Because the present invention adopts 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, the compound initiation of peroxidation (two) benzoyl, dibutyl tin laurate is catalyst vinyl long-chain unsaturated silane graft crosslinking modification T30s and is prepared the 20cN high melt strength, propylene, can make reaction uniform and stable, quality product is very high, and product stability is good.Have economy, energy consumption is low, productive rate is high, melt strength is higher, the characteristics of free from extraneous odour.
Below in conjunction with embodiment, production method of the present invention is described in further detail.
Embodiment one
One step of a kind of T30s is extruded the method for the crosslinked 20cN of preparation high melt strength, propylene, and its production stage is:
The first step is opened twin screw extruder, and 95 parts of dried polypropylene T30s are evenly fed by hopper, and screw speed is 200 to turn/min, 180 ℃ of Heating temperatures.
Second step, with 1 part 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, 0.5 part of peroxidation (two) benzoyl (being dissolved in 20 parts of acetone) mix, and are pumped into by volume pump from forcing machine the second heating module;
The 3rd step was that 2 parts of vinyl long-chain unsaturated silanes, 0.5 part of dibutyl tin laurate and 10 parts of acetone dissolve each other with mass ratio, had volume pump to pump into from forcing machine the 3rd heating module; The adjusting screw(rod) rotating speed, feed rate, volume pump liquid flow rate make each raw material simultaneous reactions complete, and the acetone reduction vaporization is reclaimed.Cooling and dicing after melt extrusion.
Because the present invention adopts 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, the compound initiation of peroxidation (two) benzoyl, dibutyl tin laurate is catalyst vinyl long-chain unsaturated silane graft crosslinking modification T30s and is prepared the 20cN high melt strength, propylene, can make reaction uniform and stable, quality product is very high, and product stability is good.Have economy, energy consumption is low, productive rate is high, melt strength is higher, the characteristics of free from extraneous odour.
Embodiment two
One step of a kind of T30s is extruded the method for the crosslinked 20cN of preparation high melt strength, propylene, and its production stage is:
The first step is opened twin screw extruder, and 98 parts of dried polypropylene T30s are evenly fed by hopper, and screw speed is 400 to turn/min, 200 ℃ of Heating temperatures.
Second step, with 2 part 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, 1 part of peroxidation (two) benzoyl (being dissolved in 100 parts of acetone) mix, and are pumped into by volume pump from forcing machine the second heating module;
The 3rd step was that 3 parts of vinyl long-chain unsaturated silanes, 1 part of dibutyl tin laurate and 20 parts of acetone dissolve each other with mass ratio, had volume pump to pump into from forcing machine the 3rd heating module; The adjusting screw(rod) rotating speed, feed rate, volume pump liquid flow rate make each raw material simultaneous reactions complete, and the acetone reduction vaporization is reclaimed.Cooling and dicing after melt extrusion.
Because the present invention adopts 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, the compound initiation of peroxidation (two) benzoyl, dibutyl tin laurate is catalyst vinyl long-chain unsaturated silane graft crosslinking modification T30s and is prepared the 20cN high melt strength, propylene, can make reaction uniform and stable, quality product is very high, and product stability is good.Have economy, energy consumption is low, productive rate is high, melt strength is higher, the characteristics of free from extraneous odour.
Embodiment three
One step of a kind of T30s is extruded the method for the crosslinked 20cN of preparation high melt strength, propylene, and its production stage is:
The first step is opened twin screw extruder, and 98 parts of dried polypropylene T30s are evenly fed by hopper, and screw speed is 300 to turn/min, 200 ℃ of Heating temperatures.
Second step, with 1.5 part 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, 0.5 part of peroxidation (two) benzoyl (being dissolved in 50 parts of acetone) mix, and are pumped into by volume pump from forcing machine the second heating module;
The 3rd step was that 5 parts of vinyl long-chain unsaturated silanes, 2 parts of dibutyl tin laurates and 50 parts of acetone dissolve each other with mass ratio, had volume pump to pump into from forcing machine the 3rd heating module; The adjusting screw(rod) rotating speed, feed rate, volume pump liquid flow rate make each raw material simultaneous reactions complete, and the acetone reduction vaporization is reclaimed.Cooling and dicing after melt extrusion.
Because the present invention adopts 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, the compound initiation of peroxidation (two) benzoyl, dibutyl tin laurate is catalyst vinyl long-chain unsaturated silane graft crosslinking modification T30s and is prepared the 20cN high melt strength, propylene, can make reaction uniform and stable, quality product is very high, and product stability is good.Have economy, energy consumption is low, productive rate is high, melt strength is higher, the characteristics of free from extraneous odour.
Embodiment four
One step of a kind of T30s is extruded the method for the crosslinked 20cN of preparation high melt strength, propylene, and its production stage is:
The first step is opened twin screw extruder, and 96 parts of dried polypropylene T30s are evenly fed by hopper, and screw speed is 300 to turn/min, 200 ℃ of Heating temperatures.
Second step, with 0.5 part 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, 0.7 part of peroxidation (two) benzoyl (being dissolved in 50 parts of acetone) mix, and are pumped into by volume pump from forcing machine the second heating module;
The 3rd step was that 1 part of vinyl long-chain unsaturated silane, 0.1 part of dibutyl tin laurate and 4 parts of acetone dissolve each other with mass ratio, had volume pump to pump into from forcing machine the 3rd heating module; The adjusting screw(rod) rotating speed, feed rate, volume pump liquid flow rate make each raw material simultaneous reactions complete, and the acetone reduction vaporization is reclaimed.Cooling and dicing after melt extrusion.
Because the present invention adopts 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, the compound initiation of peroxidation (two) benzoyl, dibutyl tin laurate is catalyst vinyl long-chain unsaturated silane graft crosslinking modification T30s and is prepared the 20cN high melt strength, propylene, can make reaction uniform and stable, quality product is very high, and product stability is good.Have economy, energy consumption is low, productive rate is high, melt strength is higher, the characteristics of free from extraneous odour.
the present invention is catalyst vinyl long-chain unsaturated silane graft crosslinking T30s with dibutyl tin laurate, so, makes reaction more thorough, and degree of crosslinking is improved, and therefore, makes the polyacrylic melt strength that finally obtains reach 20cN, in addition, the present invention adopts 2, 5-dimethyl-2, 5-bis(t-butylperoxy) hexane and peroxidation (two) benzoyl is compound as initiator, make whole preparation method's cost lower, and the polypropylene that finally obtains does not have peculiar smell, if separately with 2, 5-dimethyl-2, 5-bis(t-butylperoxy) hexane is as initiator, in preparation process, can produce very large peculiar smell, general staff all can't stand, if with independent peroxidation (two) benzoyl as initiator, the performance of at first peroxidation (two) benzoyl a little less than, secondly, the cost of peroxidation (two) benzoyl is also higher, present patent application contriver is through test of long duration, if find peroxidation (two) benzoyl and 2, 5-dimethyl-2, 5-bis(t-butylperoxy) hexane is compound suitable as initiator and proportioning, can reduce the cost of whole technique, can also remove 2, 5-dimethyl-2, the peculiar smell that 5-bis(t-butylperoxy) hexane produces.
The above is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading specification sheets of the present invention is claim of the present invention and contains.

Claims (4)

1. a cross-linking modified T30s prepares the method for HMSPP, it is characterized in that: with 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane and peroxidation (two) benzoyl is as initiator, make catalyzer with dibutyl tin laurate, catalyzed ethylene base long-chain unsaturated silane graft crosslinking modification T30s prepares the 20cN high melt strength, propylene; According to the mass fraction meter, described 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane is 0.5-2 part, described peroxidation (two) benzoyl is 0.5-1 part, described dibutyl tin laurate is 0.1-2 part, and described vinyl long-chain unsaturated silane is 1-5 part, and described T30s is 95-98 part.
2. a kind of cross-linking modified T30s as claimed in claim 1 prepares the method for HMSPP, it is characterized in that: at first described peroxidation (two) benzoyl was dissolved in the acetone of 20-100 part before adding.
3. a kind of cross-linking modified T30s as claimed in claim 1 prepares the method for HMSPP, it is characterized in that: described vinyl long-chain unsaturated silane and dibutyl tin laurate add after being dissolved in 4-50 part acetone soln again.
4. a cross-linking modified T30s prepares the method for HMSPP, it is characterized in that: comprise the following steps: the first step, unlatching twin screw extruder, the polypropylene T30s that 95-98 part is dried is evenly fed by hopper, and screw speed is that 200-400 turns/min, Heating temperature 180-200 ℃;
Second step, with 0.5-2 part 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane and 0.5-1 part peroxidation (two) benzoyl that is dissolved in acetone mix, and are pumped into by volume pump from forcing machine the second heating module;
The 3rd the step, be after 1-5 part vinyl long-chain unsaturated silane, 0.1-2 part dibutyl tin laurate and 4-50 part acetone dissolve each other, to be pumped into by volume pump from forcing machine the 3rd heating module with mass ratio; Make each raw material simultaneous reactions complete, at last the acetone reduction vaporization is reclaimed cooling and dicing after melt extrusion.
CN2013100980274A 2013-03-25 2013-03-25 Method for preparing HMSPP (High Melt Strength Polypropylene) from cross-linked and modified T30s Pending CN103159897A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104844770B (en) * 2015-04-15 2018-05-08 宁波奇红电器有限公司 A kind of refrigerator-freezer liner material and preparation method thereof
CN110183857A (en) * 2019-07-01 2019-08-30 厦门翔矽新材料有限公司 Organosilicon material, preparation method and application

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102603983A (en) * 2012-03-23 2012-07-25 陕西省轻工业研究设计院 Method for preparing polypropylene with high-melt-strength by modifying T30s through acetone solvent method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102603983A (en) * 2012-03-23 2012-07-25 陕西省轻工业研究设计院 Method for preparing polypropylene with high-melt-strength by modifying T30s through acetone solvent method

Non-Patent Citations (1)

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Title
杨明山等: "《现代工程塑料改性——理论与实践》", 31 July 2009, article "通用塑料的高性能化、精细化和功能化", pages: 126-128 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104844770B (en) * 2015-04-15 2018-05-08 宁波奇红电器有限公司 A kind of refrigerator-freezer liner material and preparation method thereof
CN110183857A (en) * 2019-07-01 2019-08-30 厦门翔矽新材料有限公司 Organosilicon material, preparation method and application

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Application publication date: 20130619