CN108148223A - A kind of flame-retarding new material for Corvic - Google Patents

A kind of flame-retarding new material for Corvic Download PDF

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Publication number
CN108148223A
CN108148223A CN201711338813.1A CN201711338813A CN108148223A CN 108148223 A CN108148223 A CN 108148223A CN 201711338813 A CN201711338813 A CN 201711338813A CN 108148223 A CN108148223 A CN 108148223A
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CN
China
Prior art keywords
parts
flame
ammonium polyphosphate
corvic
new material
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Pending
Application number
CN201711338813.1A
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Chinese (zh)
Inventor
王大可
张欣
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Xiaogan Ruxi New Material Technology Co Ltd
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Xiaogan Ruxi New Material Technology Co Ltd
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Priority to CN201711338813.1A priority Critical patent/CN108148223A/en
Publication of CN108148223A publication Critical patent/CN108148223A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/55Boron-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant

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  • 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 present invention relates to a kind of flame-retarding new materials for Corvic.Its component is not easy 100 parts of the ammonium polyphosphate being precipitated made from including, 5 15 parts of aluminium hydroxide, 10 20 parts of calcium carbonate, bicyclopentadiene close 4 12 parts of iron, 39 parts of ricinoleic acid amide hydroxypropyltrimonium chloride, 4 0.5 1.5 parts of (succinimidyl) phenyl boric acid pinacol esters.There is the flame retardant products that the present invention is produced flame retardant effect to stablize, and can reduce the pernicious gas amount that smoke delivery and polyvinyl chloride are released through burning.

Description

A kind of flame-retarding new material for Corvic
Technical field
The present invention relates to a kind of fire retardant combinations, especially a kind of to be used for fire retardant combination known to polyvinyl chloride.
Background technology
Polyvinyl chloride, English abbreviation PVC(Polyvinyl chloride), it is vinyl chloride monomer(vinyl chloride Monomer, abbreviation VCM)In initiators such as peroxide, azo-compounds;It is or anti-by free radical polymerization under light, heat effect Answer the polymer that mechanism is polymerized.Ryuron and vinyl chloride copolymer system are referred to as vinyl chloride resin.PVC was once generation The general-purpose plastics of yield maximum, is widely used general in boundary.Construction material, industrial product, daily necessities, flooring laminate, floor tile, Artificial leather, tubing, electric wire, packaging film, bottle, expanded material, sealing material, fiber etc. are widely used.Poly- Fire retardant is introduced in vinyl chloride resin, smoke amount during its burning can be reduced, strengthens the flame retardant property of Corvic, is enabled It possesses more safe and stable performance in use.
CN105462101A discloses a kind of flame Retarding Polyvinyl Chloride Plastics, which is characterized in that by following weight ratio raw material group Into:100 calcium carbonate of polyvinyl chloride raw material:5.0~6.0 talcum powder:4.5~5.5 mica powders:4.5~5.5 kaolin:4.5~ 5.5 silica:4.5~5.5 dispersed lubricants (TAS, 2A):0.5~1.5 titanate coupling agent:1.0~2.0 zinc borates: 4.5~5.5 antimony oxides:4.5~5.5.
CN106543600A discloses a kind of flame-proof polyvinyl chloride, is related to technical field of polymer materials, combination raw materials packet It includes:120~140 parts of polyvinyl chloride, 20~30 parts of eight bromo ether, 17~25 parts of hexabromocyclododecane, 12~15 parts of decabromodiphenyl oxide, 8~13 parts of ammonium polyphosphate, 5~9 parts of chlorinated paraffin, 14~22 parts of pentalyn, 7~12 parts of erucyl amide, dodecane 5~9 parts of base glycine betaine, 22~31 parts of Coconut Fatty Acid Monoethanolamide, 16~22 parts of tetrachloroquinone, 21~29 parts of antistatic agent, profit 14~21 parts of lubrication prescription, 15~23 parts of nucleating agent.
The existing fire retardant applied to Corvic uses boron flame retardant or bromide fire retardant mostly, the former Need amount to be added big, and flame retardant effect is not strong, the latter is larger for environmental pollution.
Invention content
Present invention aims at the above-mentioned technical problems in the prior art are solved, provide a kind of for polyvinyl chloride tree The flame-retarding new material of fat, it is characterised in that preparation process includes:
1. the cladding of ammonium polyphosphate
By weight, 100 parts of ammonium polyphosphate, vinyl three (2- methoxy ethoxies) silane 15-30 are added in a kettle Part, (the chloro- 2- formylethenyls of 1-) 0.0001-0.001 parts of ferrocene, 300-500 parts of chlorobenzene, the benzoyl peroxide tert-butyl ester 1-4 parts, 2-6h is reacted at 85-105 DEG C, product is filtered, washs, and drying is crushed to get to coated ammonium polyphosphate.
2. the preparation of composition
By weight, 100 parts of ammonium polyphosphate made from step 1,5-15 parts of aluminium hydroxide, calcium carbonate are added in a kettle 10-20 parts, bicyclopentadiene closes 4-12 parts of iron, 3-9 parts of ricinoleic acid amide hydroxypropyltrimonium chloride, 4- (succinimidyl) 0.5-1.5 parts of phenyl boric acid pinacol ester, is warming up to 80-100 DEG C, with the rotating speed of 150-300rpm stirring 20-60min to get to For the flame-retarding new material of Corvic.
The ammonium polyphosphate, vinyl three (2- methoxy ethoxies) silane, (the chloro- 2- formylethenyls of 1-) two cyclopentadienyl Iron, chlorobenzene, the benzoyl peroxide tert-butyl ester, ammonium polyphosphate, aluminium hydroxide, calcium carbonate, bicyclopentadiene close iron, ricinoleic acid acyl Amine hydroxypropyltrimonium chloride, 4- (succinimidyl) phenyl boric acid pinacol ester is commercial product.
The method have the advantages that:
The flame retardant products that the present invention is produced, effective flame-retardant composition ammonium polyphosphate are not easy to be precipitated, and can be stable in the presence of polychlorostyrene In vinyl, permanent performance flame retardant efficiency;Flame retardant products and the compatibility of resin are good, easily uniformly divide in resin It dissipates, while effectively reduces the discharge rate of the smoke output and pernicious gas when resin burns.
Specific embodiment
Following instance is only to further illustrate the present invention, and is not limitation the scope of protection of the invention.
Embodiment 1
The cladding of step 1. ammonium polyphosphate
In a kettle, ammonium polyphosphate 1000g, vinyl three (2- methoxy ethoxies) silane 225g, (the chloro- 2- first of 1- are added in Acyl group vinyl) ferrocene 0.5g, chlorobenzene 4000g, benzoyl peroxide tert-butyl ester 15g, in 95 DEG C of reaction 3h, product passes through Filter is washed, and drying is crushed to get to coated ammonium polyphosphate.
The preparation of step 2. composition
In a kettle, ammonium polyphosphate 1000g, aluminium hydroxide 100g, calcium carbonate 150g made from step 1, two rings penta 2 are added in Alkene closes iron 80g, ricinoleic acid amide hydroxypropyltrimonium chloride 60g, 4- (succinimidyl) phenyl boric acid pinacol ester 10g, rises Temperature is to 90 DEG C, with the rotating speed of 225rpm stirring 40min to get to the flame-retarding new material for Corvic.
Embodiment 2
The cladding of step 1. ammonium polyphosphate
In a kettle, ammonium polyphosphate 1000g, vinyl three (2- methoxy ethoxies) silane 150g, (the chloro- 2- first of 1- are added in Acyl group vinyl) ferrocene 0.1g, chlorobenzene 3000g, benzoyl peroxide tert-butyl ester 10g, in 85 DEG C of reaction 2h, product passes through Filter is washed, and drying is crushed to get to coated ammonium polyphosphate.
The preparation of step 2. composition
In a kettle, ammonium polyphosphate 1000g, aluminium hydroxide 50g, calcium carbonate 100g made from step 1, bicyclopentadiene are added in Iron 40g is closed, ricinoleic acid amide hydroxypropyltrimonium chloride 30g, 4- (succinimidyl) phenyl boric acid pinacol ester 5g is warming up to 80 DEG C, with the rotating speed of 150rpm stirring 20min to get to the flame-retarding new material for Corvic.
Embodiment 3
The cladding of step 1. ammonium polyphosphate
In a kettle, ammonium polyphosphate 1000g, vinyl three (2- methoxy ethoxies) silane 300g, (the chloro- 2- first of 1- are added in Acyl group vinyl) ferrocene 1g, chlorobenzene 5000g, benzoyl peroxide tert-butyl ester 40g, in 105 DEG C of reaction 4h, product is filtered, Washing, drying are crushed to get to coated ammonium polyphosphate.
The preparation of step 2. composition
In a kettle, ammonium polyphosphate 1000g, aluminium hydroxide 150g, calcium carbonate 200g made from step 1, two rings penta 2 are added in Alkene closes iron 120g, ricinoleic acid amide hydroxypropyltrimonium chloride 90g, 4- (succinimidyl) phenyl boric acid pinacol ester 15g, rises Temperature is to 100 DEG C, with the rotating speed of 300rpm stirring 60min to get to the flame-retarding new material for Corvic.
Comparative example 1
Step 1 is added without vinyl three (2- methoxy ethoxies) silane, and other conditions are the same as embodiment 1.
Comparative example 2
Step 1 is added without (the chloro- 2- formylethenyls of 1-) ferrocene, and other conditions are the same as embodiment 1.
Comparative example 3
Step 2 is added without ricinoleic acid amide hydroxypropyltrimonium chloride, and other conditions are the same as embodiment 1.
Comparative example 4
Step 2 is added without 4- (succinimidyl) phenyl boric acid pinacol ester, and other conditions are the same as embodiment 1.
Embodiment 4
The fire retardant combination obtained by embodiment 1-3 and comparative example 1-4 is mixed into Corvic respectively, matter Measure 6% that dosage is polyvinyl chloride raw material, the resistance that will add in embodiment 1-3 and comparative example 1-4 by standard GB/T 2406-1993 Combustion agent 5wt% is added in the Corvic downcomer mixture of standard known in the industry, after placing one month, to by GB/ T 2406-1993 detectable limit oxygen index (OI)s, and calculate its reducible Heat liberation unit.It is shown in Table 1.
Table 1:The comparison of test specimen flame retardant property that different process is made.

Claims (2)

1. a kind of flame-retarding new material for Corvic, which is characterized in that including following component and preparation process:By weight Part meter is measured, in a kettle 100 parts of ammonium polyphosphate made from addition step 1,5-15 parts of aluminium hydroxide, 10-20 parts of calcium carbonate, two Cyclopentadiene closes 4-12 parts of iron, and 3-9 parts of ricinoleic acid amide hydroxypropyltrimonium chloride, where is 4- (succinimidyl) phenyl boric acid frequency 0.5-1.5 parts of alcohol ester, is warming up to 80-100 DEG C, and 20-60min is stirred to get to for polychlorostyrene second with the rotating speed of 150-300rpm The flame-retarding new material of olefine resin.
2. a kind of flame-retarding new material for Corvic according to claim 1, which is characterized in that described is poly- The preparation method of ammonium phosphate includes the following steps:By weight, 100 parts of ammonium polyphosphate, vinyl three are added in a kettle 15-30 parts of (2- methoxy ethoxies) silane, (the chloro- 2- formylethenyls of 1-) 0.0001-0.001 parts of ferrocene, chlorobenzene 300-500 parts, 1-4 parts of the benzoyl peroxide tert-butyl ester reacts 2-6h at 85-105 DEG C, and product is filtered, washs, and dries, and breaks It is broken to get to coated ammonium polyphosphate.
CN201711338813.1A 2017-12-14 2017-12-14 A kind of flame-retarding new material for Corvic Pending CN108148223A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108912549A (en) * 2018-07-18 2018-11-30 曹佳男 A kind of highly effective flame-retardant type PVC floor and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103396629A (en) * 2013-07-15 2013-11-20 安徽省振云塑胶有限公司 Smoke-suppressing flame-retardant sound-insulating PVC (polyvinyl chloride) and preparation method thereof
CN104592675A (en) * 2014-12-26 2015-05-06 神盾防火科技有限公司 Polyvinyl chloride Grade-A flame-retardant fireproof wear-resistant wood-plastic floor material
CN105647037A (en) * 2016-03-01 2016-06-08 苏州科茂电子材料科技有限公司 Cable sheath material resistant to acid and base corrosion and preparation method of cable sheath material
CN106832416A (en) * 2016-12-20 2017-06-13 衢州普信新材料有限公司 A kind of preparation method of siliceous APP

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103396629A (en) * 2013-07-15 2013-11-20 安徽省振云塑胶有限公司 Smoke-suppressing flame-retardant sound-insulating PVC (polyvinyl chloride) and preparation method thereof
CN104592675A (en) * 2014-12-26 2015-05-06 神盾防火科技有限公司 Polyvinyl chloride Grade-A flame-retardant fireproof wear-resistant wood-plastic floor material
CN105647037A (en) * 2016-03-01 2016-06-08 苏州科茂电子材料科技有限公司 Cable sheath material resistant to acid and base corrosion and preparation method of cable sheath material
CN106832416A (en) * 2016-12-20 2017-06-13 衢州普信新材料有限公司 A kind of preparation method of siliceous APP

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108912549A (en) * 2018-07-18 2018-11-30 曹佳男 A kind of highly effective flame-retardant type PVC floor and preparation method thereof

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Application publication date: 20180612