CN105440443A - Calcium carbonate filled halogen-free flame-retardant PP material and preparation method thereof - Google Patents
Calcium carbonate filled halogen-free flame-retardant PP material and preparation method thereof Download PDFInfo
- Publication number
- CN105440443A CN105440443A CN201510953567.5A CN201510953567A CN105440443A CN 105440443 A CN105440443 A CN 105440443A CN 201510953567 A CN201510953567 A CN 201510953567A CN 105440443 A CN105440443 A CN 105440443A
- Authority
- CN
- China
- Prior art keywords
- halogen
- calcium carbonate
- free flame
- particle
- retardant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- 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
- C08K3/34—Silicon-containing compounds
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
- C08K5/523—Esters of phosphoric acids, e.g. of H3PO4 with hydroxyaryl compounds
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention relates to a preparation method of a calcium carbonate filled halogen-free flame-retardant PP material, which comprises the following components in percentage by weight: 45 to 55 wt% of calcium carbonate, 27 to 33 wt% of PP particle, 12 to 17 wt% of halogen-free flame retardant, 1 to 2 wt% of antioxidant, and 4 to 7 wt% of organic silicon, wherein the total weight percentage is 100 wt%. The preparation method comprises the following steps: (1) mixing PP particles and calcium carbonate, and blending the PP particles and calcium carbonate at a temperature of 80 DEG C in a low speed automatic metering mixer in a low speed; (2) adding an antioxidant, organic silicon, and halogen-free flame retardant through a middle speed blender, and evenly blending in a middle speed to obtain a raw material composition; (3) automatically delivering the whole raw material composition into a vertical container, heating to a temperature of 120 DEG C, vacuumizing, and carrying out plasticization under a high stirring speed; (4) automatically transferring the materials to a double screw extruder, and extruding the materials at a temperature of 220 DEG C so as to obtain the highly filled halogen-free flame-retardant PP material. The provided calcium carbonate highly filled halogen-free flame-retardant PP material can reach the UL94V2 (0.8mm) level, the hardness is high, the shore hardness can reach 100 or more, the surface is smooth, the PP material does not contain any halogen and is environment-friendly, the cost is low, and the industrial production is possible.
Description
Technical field
The invention belongs to PP field of material preparation, be specifically related to a kind of calcium carbonate-filled halogen-free flameproof PP material and preparation method thereof.
Background technology
Polypropylene is a kind of thermoplastic resin obtained by propylene polymerization.The requirements such as conventional P P material technology, cannot have the advantage that low halogen is fire-retardant with high calcium carbonate filled concurrently, and the field such as household electrical appliance, fire-resistant decoration plate has halogen-free environmental, low cost concurrently to PP material require, and fire-retardant, shrinkability is good.And the PP material of prior art cannot meet each side requirement.
This area needs to develop a kind of halogen-free environmental, low cost, the PP material that fire-retardant, shrinkability is good.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of calcium carbonate-filled halogen-free flameproof PP material, the raw materials by weight of described method comprises following component:
Carbonic acid Ca45 ~ 55wt%
PP particle 27 ~ 33wt%
Halogen-free flame retardants 12 ~ 17wt%
Oxidation inhibitor 1 ~ 2wt%
Organosilicon 4 ~ 7wt%
The mass percent sum of described raw material is 100wt%;
Described method comprises the steps:
(1) mix PP particle, calcium carbonate, one-level is blended;
(2) add oxidation inhibitor, organosilicon sunset oil, halogen-free flame retardants, secondary is blended, obtains feedstock composition after mixing;
(3) feedstock composition is heated up, carry out half plasticizing;
(4) Screw Extrusion subsequently, obtains calcium carbonate-filled halogen-free flameproof PP material.
Preferably, the particle diameter of described PP particle is 50nm ~ 100 μm, preferred 70nm ~ 10 μm, further preferred 100nm ~ 5 μm.
Preferably, the particle diameter of described calcium carbonate is 50nm ~ 100 μm, preferred 70nm ~ 10 μm, further preferred 100nm ~ 5 μm.
Preferably, described halogen-free flame retardants comprises nitrogenated flame retardant and/or phosphorus flame retardant.
Preferably, described nitrogenated flame retardant is trimeric cyanamide.
Preferably, described phosphorus flame retardant is selected from the combination of any a kind or at least 2 kinds in phosphoric acid ester, phosphorous acid ester, organophosphate, preferred polyphosphoric acid amine and/or Tritolyl Phosphate.
Preferably, described organosilicon is selected from vapor phase process three oxygen silicon, four oxygen silicon or five oxygen silicon.
Preferably, described half plasticization temperature is 115 ~ 135 DEG C, and the time is 3 ~ 6min; Preferably 130 DEG C, 5min.
As optimal technical scheme, the raw materials by weight of the preparation method of calcium carbonate-filled halogen-free flameproof PP material of the present invention comprises following component:
Calcium carbonate 50wt%
PP particle 30wt%
Halogen-free flame retardants 15wt%
Oxidation inhibitor 1wt%
Organosilicon 4wt%
Described method comprises the steps:
(1) mix PP particle, calcium carbonate, one-level is blended;
(2) add oxidation inhibitor, organosilicon sunset oil, halogen-free flame retardants, secondary is blended, obtains feedstock composition after mixing;
(3) feedstock composition is heated up 130 DEG C, carry out half plasticizing 5min;
(4) Screw Extrusion subsequently, obtains calcium carbonate-filled halogen-free flameproof PP material.
The temperature of Screw Extrusion is not specifically limited, and typical but non-limitingly comprises 200 DEG C, 210 DEG C or 220 DEG C etc.
As alternatives, the raw materials by weight of the preparation method of calcium carbonate-filled halogen-free flameproof PP material of the present invention comprises following component: the mass percent sum of carbonic acid Ca45 ~ 55wt%, PP particle 27 ~ 33wt%, halogen-free flame retardants 12 ~ 17wt%, oxidation inhibitor 1 ~ 2wt%, organosilicon 4 ~ 7wt%, described raw material is 100wt%; Described method comprises the steps: (1) mixing PP particle, calcium carbonate, blended by low speed (10rpm) automatic gauge mixing tank 80 DEG C of low speed of heating; (2) again add oxidation inhibitor, organosilicon, halogen-free flame retardants by middling speed (100rpm) stirrer, middling speed is blended evenly, obtain feedstock composition; (3) all composition automatizations input vertical vessel is heated up 120 DEG C carry out stirrings and plastify; (4) material automatically proceeds to twin screw design temperature and extrudes at 220 DEG C, obtains highly to fill halogen-free flameproof PP material.
Two of the object of the invention is to provide a kind of calcium carbonate-filled halogen-free flameproof PP material, and described calcium carbonate-filled halogen-free flameproof PP material is obtained by the preparation method one of object Suo Shu.
Compared with prior art, the present invention has following beneficial effect:
Calcium carbonate-filled halogen-free flameproof PP material flame retardant type provided by the invention is good, and can reach UL94V2 (0.8mm) rank, hardness is high, at shore hardness more than 100, and smooth surface, halogen-free environmental.
Embodiment
Technical scheme of the present invention is further illustrated below by embodiment.
Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
A calcium carbonate-filled halogen-free flameproof PP material, the raw materials by weight of its preparation method comprises following component:
Calcium carbonate 50wt%
PP particle 30wt%
Halogen-free flame retardants 15wt%
Oxidation inhibitor 1wt%
Vapor phase process three silicon oxide 4wt%
Described method comprises the steps:
(1) mix high crystallization PP particle (100nm ~ 3 μm), calcium carbonate (100nm ~ 3 μm), one-level is blended;
(2) add antioxidant 1010, vapor phase process three silicon oxide, Tritolyl Phosphate, secondary is blended, obtains feedstock composition after mixing;
(3) feedstock composition is heated up 120 DEG C, carry out half plasticizing 5min;
(4) Screw Extrusion subsequently, obtains wear-resisting stable PP electroplating substrate.
Performance test: after measured, shore D hardness is 110, and flame retardant rating is UL94V2 (0.8mm).
Embodiment 2
A calcium carbonate-filled halogen-free flameproof PP material, the raw materials by weight of its preparation method comprises following component:
Calcium carbonate 46wt%
PP particle 33wt%
Halogen-free flame retardants 12wt%
Oxidation inhibitor 2wt%
Vapor phase process three silicon oxide 7wt%
Described method comprises the steps:
(1) mix high crystallization PP particle (100nm ~ 3 μm), calcium carbonate (100nm ~ 3 μm), one-level is blended;
(2) add antioxidant 1010, vapor phase process three silicon oxide, Tritolyl Phosphate, secondary is blended, obtains feedstock composition after mixing;
(3) feedstock composition is heated up 120 DEG C, carry out half plasticizing 5min;
(4) Screw Extrusion subsequently, obtains wear-resisting stable PP electroplating substrate.
Performance test: after measured, shore D hardness is 100, and flame retardant rating is UL94V2 (0.8mm).
Embodiment 3
A calcium carbonate-filled halogen-free flameproof PP material, the raw materials by weight of its preparation method comprises following component:
Calcium carbonate 55wt%
PP particle 27wt%
Halogen-free flame retardants 12wt%
Oxidation inhibitor 1wt%
Vapor phase process three silicon oxide 5wt%
Described method comprises the steps:
(1) mix high crystallization PP particle (100nm ~ 3 μm), calcium carbonate (100nm ~ 3 μm), one-level is blended;
(2) add antioxidant 1010, vapor phase process three silicon oxide, Tritolyl Phosphate, secondary is blended, obtains feedstock composition after mixing;
(3) feedstock composition is heated up 120 DEG C, carry out half plasticizing 5min;
(4) Screw Extrusion subsequently, obtains wear-resisting stable PP electroplating substrate.
Performance test: after measured, shore D hardness is 105, and flame retardant rating is UL94V2 (0.8mm).
Applicant states, the present invention illustrates processing method of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned processing step, does not namely mean that the present invention must rely on above-mentioned processing step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of raw material selected by the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. a preparation method for calcium carbonate-filled halogen-free flameproof PP material, is characterized in that, the raw materials by weight of described method comprises following component:
Carbonic acid Ca45 ~ 55wt%
PP particle 27 ~ 33wt%
Halogen-free flame retardants 12 ~ 17wt%
Oxidation inhibitor 1 ~ 2wt%
Organosilicon 4 ~ 7wt%
The mass percent sum of described raw material is 100wt%;
Described method comprises the steps:
(1) mix PP particle, calcium carbonate, one-level is blended;
(2) add oxidation inhibitor, organosilicon, halogen-free flame retardants, secondary is blended, obtains feedstock composition after mixing;
(3) feedstock composition is heated up, carry out half plasticizing;
(4) Screw Extrusion subsequently, obtains calcium carbonate-filled halogen-free flameproof PP material.
2. the method for claim 1, is characterized in that, the particle diameter of described PP particle is 50nm ~ 100 μm, preferred 70nm ~ 10 μm, further preferred 100nm ~ 5 μm.
3. method as claimed in claim 1 or 2, it is characterized in that, the particle diameter of described calcium carbonate is 50nm ~ 100 μm, preferred 70nm ~ 10 μm, further preferred 100nm ~ 5 μm.
4. the method as described in one of claims 1 to 3, is characterized in that, described halogen-free flame retardants comprises nitrogenated flame retardant and/or phosphorus flame retardant.
5. the method as described in one of Claims 1 to 4, is characterized in that, described nitrogenated flame retardant is trimeric cyanamide.
6. the method as described in one of Claims 1 to 5, is characterized in that, described phosphorus flame retardant is selected from the combination of any a kind or at least 2 kinds in phosphoric acid ester, phosphorous acid ester, organophosphate, preferred polyphosphoric acid amine and/or Tritolyl Phosphate.
7. the method as described in one of claim 1 ~ 6, is characterized in that, described organosilicon is selected from vapor phase process three oxygen silicon, four oxygen silicon or five oxygen silicon.
8. the method as described in one of claim 1 ~ 7, is characterized in that, described half plasticization temperature is 115 ~ 135 DEG C, and the time is 3 ~ 6min; Preferably 130 DEG C, 5min.
9. the method as described in one of claim 1 ~ 8, is characterized in that, the raw materials by weight of described method comprises following component:
Calcium carbonate 50wt%
PP particle 30wt%
Halogen-free flame retardants 15wt%
Oxidation inhibitor 1wt%
Organosilicon 4wt%
Described method comprises the steps:
(1) mix PP particle, calcium carbonate, one-level is blended;
(2) add oxidation inhibitor, organosilicon sunset oil, halogen-free flame retardants, secondary is blended, obtains feedstock composition after mixing;
(3) feedstock composition is heated up 130 DEG C, carry out half plasticizing 5min;
(4) Screw Extrusion subsequently, obtains calcium carbonate-filled halogen-free flameproof PP material.
10. a calcium carbonate-filled halogen-free flameproof PP material, is characterized in that, described calcium carbonate-filled halogen-free flameproof PP material is obtained by the preparation method one of claim 1 ~ 9 Suo Shu.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510953567.5A CN105440443B (en) | 2015-12-17 | 2015-12-17 | Calcium carbonate-filled halogen-free flameproof PP materials and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510953567.5A CN105440443B (en) | 2015-12-17 | 2015-12-17 | Calcium carbonate-filled halogen-free flameproof PP materials and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105440443A true CN105440443A (en) | 2016-03-30 |
| CN105440443B CN105440443B (en) | 2017-12-12 |
Family
ID=55551112
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510953567.5A Active CN105440443B (en) | 2015-12-17 | 2015-12-17 | Calcium carbonate-filled halogen-free flameproof PP materials and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105440443B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070838A (en) * | 2010-12-31 | 2011-05-25 | 东莞市赛泽康纳米科技有限公司 | Nano polypropylene composite material |
| CN103756136A (en) * | 2013-12-30 | 2014-04-30 | 浙江普利特新材料有限公司 | Halogen-free flame retardant polypropylene composition and preparation method thereof |
-
2015
- 2015-12-17 CN CN201510953567.5A patent/CN105440443B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102070838A (en) * | 2010-12-31 | 2011-05-25 | 东莞市赛泽康纳米科技有限公司 | Nano polypropylene composite material |
| CN103756136A (en) * | 2013-12-30 | 2014-04-30 | 浙江普利特新材料有限公司 | Halogen-free flame retardant polypropylene composition and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105440443B (en) | 2017-12-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101570631B (en) | High-heat resistance halogen-free fire-retarding polyphenylether and polystyrene composite and preparation method thereof | |
| CN101389696B (en) | Halogen-free flame retardant compositions, thermoplastic compositions comprising the same and methods of producing the compositions | |
| CN102850661B (en) | Halogen-free flame-retardant PP/polyester alloy and preparation method thereof | |
| CN103030886B (en) | Transparent polypropylene and preparation method thereof | |
| CN105283514B (en) | Carbon black, conductive resin composition and electrode mixing material | |
| CN101824182B (en) | Halogen-free expansion type flame-retardant thermoplastic elastomer composition | |
| CN102585378B (en) | High heat resistant glass fiber enhanced halogen-free flame retardant polypropylene and preparation method thereof | |
| CN104479353B (en) | Novel halogen-free flame-retardant composition, halogen-free flame-retardant PBT engineering plastic composite material and preparation method thereof | |
| CN101857712B (en) | Halogen-free flame-retardant ABS/PET alloy and preparation method thereof | |
| CN104250434B (en) | A kind of phosphorous-nitrogen system bittern-free flame-retardant polylactic acid material | |
| CN105111583A (en) | Halogen-free flame-retardant polypropylene micro foaming material and preparation method thereof | |
| CN101341211A (en) | Flameretardant thermoplastic resin composition | |
| TW201006887A (en) | Flame retardant polyurethane composition | |
| JP2022505519A (en) | Flame-retardant HIPS material and its manufacturing method | |
| CN104693760A (en) | Blended alloy of polycarbonate and polybutylene terephthalate | |
| CN104194302B (en) | A kind of ABS deflagration level Masterbatch | |
| CN104140588A (en) | Multicomponent halogen-free flame-retardant master batch and preparation method | |
| CN104725797A (en) | Method for preparing flame-retardant plastic composite material | |
| CN105440443A (en) | Calcium carbonate filled halogen-free flame-retardant PP material and preparation method thereof | |
| CN103360681B (en) | Halogen-free flame retardant highlight polypropylene and preparation method thereof | |
| CN106519653B (en) | A kind of Flameproof polyamide and preparation method thereof | |
| CN104744772A (en) | Glass fiber reinforced polyethylene powder | |
| CN104861471A (en) | PTT toughening flame retardation master batch and preparation method therefor | |
| CN102796359B (en) | Preparation method of halogen-free heat-resistant flame-retardant ABS/PC alloy | |
| CN104177824A (en) | Novel nitrogen-phosphorus system halogen-free flame-retardant nylon 6 and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PP01 | Preservation of patent right |
Effective date of registration: 20230626 Granted publication date: 20171212 |
|
| PP01 | Preservation of patent right |