CN107383597A - A kind of preparation method of diatomite modified polypropylene flame redardant - Google Patents
A kind of preparation method of diatomite modified polypropylene flame redardant Download PDFInfo
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- CN107383597A CN107383597A CN201710609362.4A CN201710609362A CN107383597A CN 107383597 A CN107383597 A CN 107383597A CN 201710609362 A CN201710609362 A CN 201710609362A CN 107383597 A CN107383597 A CN 107383597A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of diatomite modified polypropylene flame redardant, diatomite that the present invention adds etc. can effectively improve the mechanical properties such as surface strength, the hardness of finished-product material, it is blended with APP, effectively raise the area of burning carbon-coating, the effect of good gas phase barrier is served, improves the fire retardant performance of finished product.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of diatomite modified polypropylene flame redardant.
Background technology
Silane fire retardant mainly includes inorganic silicon and the class of organosilicon two, wherein inorganic silicon materials include silica, glass
Glass etc., among the field used as filler, these fire retardants are using relatively common.It is more and more with the progress of research and development
Inorganic alkane flame retardant systems be developed, what is be currently known has：The low melting point glass such as silica, glass fibre, micropore glass
Glass, stannic chloride, hydration silicon compound, silicate polyphosphoric acid, siloxanes boron etc..Inorganic silicon-series five-retardant it is main the defects of
In itself is very poor with the compatibility of base material, result in using upper problems, compatibility aspect, can generally use micron
Level or nano level micronizing, and tackle the methods of fine surface treatment.Also a kind of silicon-containing polymer, it is referred to as
INSTINCT FLAME RETARDANT POLYMERS containing alkane, be using polymerization, grafting, crosslinking technological etc., at the position such as the main chain of high-polymer molecular or side chain,
Siliceous group (such as siloxy etc.) is imported, can be to obtain INSTINCT FLAME RETARDANT POLYMERS containing alkane；This kind of material is quite outstanding, table
Reveal fabulous fire resistance, and energy high temperature resistant, there is antioxygenic property, nonflammable, in addition, this kind of material is high poly-
Thing also has good moisture-proof, and the flexibility of its strand is good, and obtain part improvement in addition is also manifested by other aspects,
For example process (because strand has compliance, the processing mechanical property to material can be improved), physics characteristic so that its
Especially anti-oxidant, energy high temperature resistant, Silicone-containing Flame Retardant is used in conjunction with the fire retardant of traditional type (or some non-flame resistant materials)
When, the complementarity of cooperative flame retardant effect and two sides, significantly showed, and its adaptability is comparatively more
Extensively, organic silicon fibre retardant with conventional flame retardant and used time, during integral combustion is carried out, under both mutually promote
The protective layer of siliceous charing can be formed.It is this kind of because its structure is very fine and close and property is stable compared with conventional layer of charcoal
The oxidation resistance that layer of charcoal is brought, and be substantially improved therewith；And the supply of oxygen can be broken off, and show quite remarkable
Heat-insulated smoke suppressing effect, dissolved drip this phenomena such as be also that can be avoided by occurring, so as to obtain the fire retardation of Synergistic because
The addition of organic silicon fibre retardant, also changed therewith by the performance of fire proofing, show processing and forming, mechanical performance, heat resistance
Etc., it can also be improved accordingly；
In recent years, it is more and more to be related to the fire-retardant research of Silicone-containing Flame Retardant, Silicone-containing Flame Retardant is just efficient fire-retardant with it
Property, environmentally friendly property, particularly to performance impact it is very small the characteristics of and become hot topic research object.To being at present
Only, researchers explored numerous species Silicone-containing Flame Retardant be applied to polyacrylic flame-retardant system in, silicide-comprising
The fire-retardant reason of compound is solidifying phase fire retardant mechanism, that is in burning silicon-containing compound to material surface Migration And Concentration into charcoal,
It is this to protect the transmission that layer of charcoal has completely cut off air and heat so as to play fire retardation.
In the last few years, more scientific workers took up to probe into the fire retardant mechanism of polymer from microcosmic angle, ground
Study carefully the change probed into from the surface combustion phenomenon of macroscopic view on molecular level, this has to silicon-containing polymer Flame Retardant Mechanism
Important breakthrough, but the compatibility between traditional Methyl Hydrogen Polysiloxane Fluid and polypropylene is poor so that composite mixing is uneven,
Reduce the stability_intensity of finished composite material.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of diatomite modified polypropylene flame redardant
Preparation method.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of diatomite modified polypropylene flame redardant, comprises the following steps：
(1) 1, the 2- methylimidazoles of 0.4-1 parts by weight are taken, are added in the absolute ethyl alcohol of 10-14 times of its weight, are stirred
Uniformly, aphthenic acids lithium, the tetramethyl disiloxane of 3-4 parts by weight of 0.1-0.2 parts by weight are added, is incubated and stirs at 50-60 DEG C
20-30 minutes are mixed, obtain silanol dispersion liquid；
(2) beta-hydroxy alkylamide of 0.6-1 parts by weight is taken, is added in the deionized water of 7-10 times of its weight, stirring is equal
It is even, obtain amide solution；
(3) diatomite of 13-20 parts by weight, the dithio-salicylic acid of 1-2 parts by weight, the ammonium hydrogen carbonate of 2-3 parts by weight are taken
Mixing, is sent in Muffle furnace, and 20-30 minutes are heated at 110-120 DEG C, and it is 50-60 DEG C to reduce temperature, is added to above-mentioned acyl
In amine aqueous solution, insulated and stirred 4-10 minutes, diatomite dispersion liquid is obtained；
(4) fatty acid polyethylene glycol ester of 0.7-1 parts by weight is taken, is added in the dimethylformamide of 4-7 times of its weight,
Stir, add the APP of 1-2 parts by weight, stir, obtain alcohol ester amide solution；
(5) silanol dispersion liquid is taken, is sent in reactor, the acrylic acid of 10-12 parts by weight is added dropwise, is added after being added dropwise
Enter the platinum dioxide of 0.1-0.3 parts by weight, be passed through nitrogen, the insulation reaction 10-15 hours at 40-50 DEG C, discharging, with above-mentioned silicon
Diatomaceous earth dispersion liquid is mixed, and ultrasonic 20-30 minutes, filters, and precipitation is washed, air drying, obtains organic siloxane modified diatomite；
(6) above-mentioned organic siloxane modified diatomite is taken, is added in alcohol ester amide solution, adds 120-130 parts by weight
Polypropylene, the calcium stearate of 2-3 parts by weight, the insulated and stirred 1-2 hours at 90-95 DEG C, discharge, filtering, will precipitation washing,
Dried completely at 60-70 DEG C of vacuum, produce the diatomite modified polypropylene flame redardant.
Advantages of the present invention：
The present invention mixes acrylic acid with silanol dispersion liquid, using platinum dioxide as catalyst, by acrylic acid and tetramethyl
Disiloxane mixes, and the C=O bond of carbon-carbon double bond and tetramethyl disiloxane present in acrylic acid could be formed with being total to for effect
Yoke, while using diatomite dispersion liquid as solvent while conjugation reaction, obtained diatomite is effectively organised, improved
Compatibility of the diatomite between polymer, improve the stability_intensity of finished product；
Diatomite that the present invention adds etc. can effectively improve the mechanical properties such as surface strength, the hardness of finished-product material,
It is blended with APP, effectively raises the area of burning carbon-coating, is served the effect of good gas phase barrier, improve into
The fire retardant performance of product.
Embodiment
Embodiment 1
A kind of preparation method of diatomite modified polypropylene flame redardant, comprises the following steps：
(1) 1, the 2- methylimidazoles of 0.4 parts by weight are taken, is added in the absolute ethyl alcohol of 14 times of its weight, stirs,
Aphthenic acids lithium, the tetramethyl disiloxane of 3 parts by weight of 0.1 parts by weight are added, insulated and stirred 20 minutes, obtain silane at 50 DEG C
Alcohol dispersion liquid；
(2) beta-hydroxy alkylamide of 0.6 parts by weight is taken, is added in the deionized water of 10 times of its weight, is stirred, obtain
Amide solution；
(3) the ammonium hydrogen carbonate mixing of the diatomite of 13 parts by weight, the dithio-salicylic acid of 1 parts by weight, 2 parts by weight is taken, is sent
Enter into Muffle furnace, heated 20 minutes at 120 DEG C, it is 60 DEG C to reduce temperature, is added in above-mentioned amide solution, insulated and stirred
4 minutes, obtain diatomite dispersion liquid；
(4) fatty acid polyethylene glycol ester of 0.7 parts by weight is taken, is added in the dimethylformamide of 4 times of its weight, is stirred
Uniformly, the APP of 1 parts by weight is added, stirs, obtains alcohol ester amide solution；
(5) silanol dispersion liquid is taken, is sent in reactor, the acrylic acid of 10 parts by weight is added dropwise, is added after being added dropwise
The platinum dioxide of 0.1 parts by weight, is passed through nitrogen, insulation reaction 10 hours at 40 DEG C, discharging, is mixed with above-mentioned diatomite dispersion liquid
Close, ultrasound 20 minutes, filter, precipitation is washed, air drying, obtains organic siloxane modified diatomite；
(6) above-mentioned organic siloxane modified diatomite is taken, is added in alcohol ester amide solution, adds the poly- of 120 parts by weight
The calcium stearate of propylene, 2 parts by weight, insulated and stirred 1 hour at 95 DEG C, discharge, filtering, precipitation is washed, at 60 DEG C of vacuum
Dry completely, produce the diatomite modified polypropylene flame redardant.
Embodiment 2
(1) 1, the 2- methylimidazoles of 1 parts by weight are taken, is added in the absolute ethyl alcohol of 14 times of its weight, is stirred, add
Enter aphthenic acids lithium, the tetramethyl disiloxane of 4 parts by weight of 0.2 parts by weight, insulated and stirred 30 minutes, obtain silanol at 60 DEG C
Dispersion liquid；
(2) beta-hydroxy alkylamide of 1 parts by weight is taken, is added in the deionized water of 10 times of its weight, is stirred, obtain acyl
Amine aqueous solution；
(3) the ammonium hydrogen carbonate mixing of the diatomite of 20 parts by weight, the dithio-salicylic acid of 2 parts by weight, 3 parts by weight is taken, is sent
Enter into Muffle furnace, heated 30 minutes at 120 DEG C, it is 60 DEG C to reduce temperature, is added in above-mentioned amide solution, insulated and stirred
10 minutes, obtain diatomite dispersion liquid；
(4) fatty acid polyethylene glycol ester of 1 parts by weight is taken, is added in the dimethylformamide of 7 times of its weight, stirring is equal
It is even, the APP of 2 parts by weight is added, stirs, obtains alcohol ester amide solution；
(5) silanol dispersion liquid is taken, is sent in reactor, the acrylic acid of 12 parts by weight is added dropwise, is added after being added dropwise
The platinum dioxide of 0.3 parts by weight, is passed through nitrogen, insulation reaction 15 hours at 50 DEG C, discharging, is mixed with above-mentioned diatomite dispersion liquid
Close, ultrasound 30 minutes, filter, precipitation is washed, air drying, obtains organic siloxane modified diatomite；
(6) above-mentioned organic siloxane modified diatomite is taken, is added in alcohol ester amide solution, adds the poly- of 130 parts by weight
The calcium stearate of propylene, 3 parts by weight, insulated and stirred 2 hours at 95 DEG C, discharge, filtering, precipitation is washed, at 70 DEG C of vacuum
Dry completely, produce the diatomite modified polypropylene flame redardant.
Performance test：
The UL-94 of the diatomite modified anti-flaming polypropylene material particle of the present invention is V-O ranks, and maximum HRR is
340-370KW/m2；
The UL-94 of virgin pp material particles is V-1 ranks, and maximum HRR is 460-480KW/m2；
As can be seen that polypropylene material of the present invention has higher fire retardant performance.
Claims (1)
1. a kind of preparation method of diatomite modified polypropylene flame redardant, it is characterised in that comprise the following steps：
(1) 1, the 2- methylimidazoles of 0.4-1 parts by weight are taken, are added in the absolute ethyl alcohol of 10-14 times of its weight, stirring is equal
It is even, add aphthenic acids lithium, the tetramethyl disiloxane of 3-4 parts by weight of 0.1-0.2 parts by weight, the insulated and stirred at 50-60 DEG C
20-30 minutes, obtain silanol dispersion liquid；
(2) beta-hydroxy alkylamide of 0.6-1 parts by weight is taken, is added in the deionized water of 7-10 times of its weight, stirs, obtain
Amide solution；
(3) the ammonium hydrogen carbonate mixing of the diatomite of 13-20 parts by weight, the dithio-salicylic acid of 1-2 parts by weight, 2-3 parts by weight is taken,
It is sent in Muffle furnace, 20-30 minutes is heated at 110-120 DEG C, it is 50-60 DEG C to reduce temperature, and it is molten to be added to above-mentioned acid amides
In liquid, insulated and stirred 4-10 minutes, diatomite dispersion liquid is obtained；
(4) fatty acid polyethylene glycol ester of 0.7-1 parts by weight is taken, is added in the dimethylformamide of 4-7 times of its weight, is stirred
Uniformly, the APP of 1-2 parts by weight is added, stirs, obtains alcohol ester amide solution；
(5) silanol dispersion liquid is taken, is sent in reactor, the acrylic acid of 10-12 parts by weight is added dropwise, is added after being added dropwise
The platinum dioxide of 0.1-0.3 parts by weight, is passed through nitrogen, the insulation reaction 10-15 hours at 40-50 DEG C, discharging, with above-mentioned diatom
Native dispersion liquid mixing, ultrasonic 20-30 minutes, filters, precipitation is washed, air drying, obtains organic siloxane modified diatomite；
(6) above-mentioned organic siloxane modified diatomite is taken, is added in alcohol ester amide solution, adds the poly- of 120-130 parts by weight
The calcium stearate of propylene, 2-3 parts by weight, the insulated and stirred 1-2 hours at 90-95 DEG C, discharge, filtering, precipitation is washed, vacuum
Dried completely at 60-70 DEG C, produce the diatomite modified polypropylene flame redardant.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710609362.4A CN107383597A (en) | 2017-07-24 | 2017-07-24 | A kind of preparation method of diatomite modified polypropylene flame redardant |
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| CN201710609362.4A CN107383597A (en) | 2017-07-24 | 2017-07-24 | A kind of preparation method of diatomite modified polypropylene flame redardant |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559133A (en) * | 2018-04-20 | 2018-09-21 | 南京工业大学 | Preparation method of diatomite-based inorganic-organic hybrid flame retardant |
| CN116751075A (en) * | 2023-06-14 | 2023-09-15 | 福建省鑫森炭业股份有限公司 | Active carbon ceramic composite filter element and manufacturing method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508809A (en) * | 2009-03-18 | 2009-08-19 | 四川大学 | Halogen-free expansion type flame-proof polyolefin composite material |
| CN103073788A (en) * | 2012-12-20 | 2013-05-01 | 华南理工大学 | Weather-resistant moisture-resistant halogen-free flame-retardant polypropylene mixture and preparation method thereof |
-
2017
- 2017-07-24 CN CN201710609362.4A patent/CN107383597A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508809A (en) * | 2009-03-18 | 2009-08-19 | 四川大学 | Halogen-free expansion type flame-proof polyolefin composite material |
| CN103073788A (en) * | 2012-12-20 | 2013-05-01 | 华南理工大学 | Weather-resistant moisture-resistant halogen-free flame-retardant polypropylene mixture and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559133A (en) * | 2018-04-20 | 2018-09-21 | 南京工业大学 | Preparation method of diatomite-based inorganic-organic hybrid flame retardant |
| CN116751075A (en) * | 2023-06-14 | 2023-09-15 | 福建省鑫森炭业股份有限公司 | Active carbon ceramic composite filter element and manufacturing method thereof |
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Application publication date: 20171124 |
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