CN103012851A - Preparation method of superfine modified brucite flame retardant and application of superfine modified brucite flame-retardant to PVC (Polyvinyl Chloride) cable material - Google Patents
Preparation method of superfine modified brucite flame retardant and application of superfine modified brucite flame-retardant to PVC (Polyvinyl Chloride) cable material Download PDFInfo
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- CN103012851A CN103012851A CN2012105799721A CN201210579972A CN103012851A CN 103012851 A CN103012851 A CN 103012851A CN 2012105799721 A CN2012105799721 A CN 2012105799721A CN 201210579972 A CN201210579972 A CN 201210579972A CN 103012851 A CN103012851 A CN 103012851A
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- Prior art keywords
- preparation
- retardant
- brucite
- superfine
- superfine modified
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Graft Or Block Polymers (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses a preparation method of a superfine modified brucite flame retardant, a cable material prepared by using the flame retardant and a preparation method of the cable material. The preparation method of the superfine modified brucite flame retardant comprises the following steps of: carrying out preprocessing, namely screening and drying, on natural brucite, crushing the dried brucite into 3-5mu m granules and putting the granules into superfine crushing equipment; putting a monomer or prepolymer, an initiator, an activating agent, a modified additive and the like to a spraying and metering device in sequence according to proportions and then spaying the mixture onto the surface of the granules in the superfine crushing equipment; and controlling the reaction temperature to be 60-150 DEG C and the superfine crushing time to be 20-60min to prepare the in-situ polymerized modified brucite flame retardant. The superfine modified brucite flame retardant is excellent in flame retardant effect; and the prepared cable material can be applied to a PVC cable.
Description
Technical field
The present invention relates to a kind of preparation method of fire retardant, also relate to a kind of superfine modified ore deposit method brucite that utilizes and be the CABLE MATERIALS of fire retardant preparation, this CABLE MATERIALS can be applicable in the PVC cable.
Technical background
Along with the develop rapidly of economy, domestic and international fire safety standard is increasingly stringent also, the usage quantity rapid growth of plastics, rubber etc., and electric wire all obtains a wide range of applications in each large industry, field.But the goods such as electric wire are owing to working under high pressure, heating, discharging condition for a long time, in case presence of fire just produces a large amount of smog and toxic gas, cause huge financial losses and loss of life and personal injury, in numerous Application Areass, the demand of the low-smoke halogen-free cable of high temperature resistant, good weatherability is day by day urgent.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of superfine modified ore deposit method brucite flame-retardant agent, and the application of this fire retardant in the PVC CABLE MATERIALS, use the CABLE MATERIALS of the present invention's preparation have high temperature resistant, intensity is high, the characteristics such as low smoke and zero halogen during burning.
To achieve these goals, the present invention adopts following technical scheme:
Superfine modified brucite flame-retardant agent is characterized in that: this fire retardant adopts the preparation of in-situ polymerization surface treatment method, and each raw materials quality umber is:
100 parts of brucites
Monomer or performed polymer 2-10 part
Initiator 0.02-1 part
Activator 0.5-5 part
Modified additive 0-10 part
Solvent 10-30 part.
The concrete steps of processing are:
(a) natural brucite is carried out pre-treatment, comprise screening, drying treatment, and be crushed to 3-5 μ m pellet, and drop in the research of super-pine crush equipment.
(b) monomer or performed polymer, initiator, activator, modified additive etc. are successively packed in proportion in the spraying measuring apparatus, spray into pellet surface in the ultrafine crusher.
(c) the control temperature of reaction is 60-150 ℃, and the superfine grinding time prepares in-situ polymerization modification brucite powder fire retardant of the present invention at 20-60min.
Described brucite is natural brucite, is also referred to as brucite, and main component is magnesium hydroxide, and content is more than 94%.
Described research of super-pine crush equipment refers to machinery mill or impact grinding, and powder granularity can be at the 1250-2500 order.
Described monomer, performed polymer are esters of acrylic acids, co polystyrene type, vinyl cyanide type and maleimide type, tetrafluoroethylene or tetrafluoroethylene/comonomer; Initiator is selected maleic anhydride, peroxycarbonates, ketone peroxide, peroxidation diacyl, the group of organic hydroperoxide and organic peroxy ester.
That described activator is selected is silicone based, rare earth organism, aluminate coupling agent, titanate coupling agent, acid phosphorous acid ester coupling agent, aluminium/titanium composite coupler, phenolate, inorganic acid salt, sulfonate.
Described properties-correcting agent is one or more mixing in silicone based, rare earth organism, diphenyl phosphate, triphenylphosphate, di(2-ethylhexyl)phosphate benzene toluene ester, ammonium polyphosphate, phosphoric acid Resorcino diphenyl ester, melamine phosphate, phenyl-phosphonic acid dimethyl ester, dimethyl methyl phosphonate, ammonium pentaborate, sodium metaborate, ammonium borofluoride, barium metaborate, zinc borate and the coating red phosphorus.
Described solvent is one or both mixing in acetone, the ethanol etc.
Use above-mentioned superfine modified brucite flame-retardant agent to be the PVC CABLE MATERIALS of fire retardant, mainly formed by base-material, fire retardant, retardant synergist, softening agent, stablizer, it is characterized in that: described base-material is the PVC(polyvinyl chloride (PVC) RESINS) with the EVA(vinyl-vinyl acetate copolymer) mixture, described fire retardant is that above-mentioned employing in-situ polymerization surface treatment method prepares superfine modified brucite flame-retardant agent, described retardant synergist is zinc borate, described softening agent is Octyl adipate and UV light absorber, and described stablizer is calcium-zinc composite stabilizing agent.
The preparation method of this PVC CABLE MATERIALS, may further comprise the steps: PVC and EVA blend is even, add the in-situ polymerization surface treatment method and prepare superfine modified flame retardant of magnesium hydroxide, retardant synergist, softening agent, stablizer, mixing under the normal temperature, carry out high-speed kneading at 80-110 ℃, drop into that twin screw extruder is mixing, granulation, the control temperature obtains this PVC CABLE MATERIALS at 130-180 ℃ again.
Flame retardant effect of the present invention is excellent, and the CABLE MATERIALS that makes can be applicable in the PVC cable.
Embodiment
Specify the present invention below in conjunction with embodiment, but embodiments of the present invention are not limited to this.
Following embodiment is superfine modified brucite flame-retardant agent.
Embodiment 1:
100 parts of brucites
6 parts of monomer or performed polymers
0.25 part of initiator
5 parts in activator
1.5 parts of modified additives
15 parts of solvents
Embodiment 2:
100 parts of brucites
8 parts of monomer or performed polymers
0.2 part of initiator
5 parts in activator
1.5 parts of modified additives
15 parts of solvents.
Superfine modified brucite flame-retardant agent is applied to the Application Example of PVC CABLE MATERIALS:
Application Example 1:
(1) raw materials pretreatment: the water intaking magnesite is raw material, obtains the natural brucite ore deposit that content is high, whiteness is good by artificial selection or machine screening, and whiteness is more than 90%, and magnesium hydroxide content is the natural brucite more than 94%; And become 5-10 μ m pellet through the broken crusher machine in Hubei Province;
(2) pulverize modification: in impact grinding, drop into the broken good pellet 200KG of crusher machine in Hubei Province, start pulverizer, in the spraying measuring apparatus, add 12 KG vinylbenzene simultaneously, 0.5 KG benzoyl peroxide, 30KG ethanol, stir, add successively again 10KG silane coupling agent, 3KG triphenylphosphate, mix, spray in the impact grinding cavity, drench on the pellet surface, add in the 15min, make the brucite powder temperature remain on 90 ℃, insulation reaction 40min, then discharging makes in-situ polymerization brucite powder fire retardant.
(3) 65 weight part PVC and 35 parts of EVA blend are even, add 20 parts of superfine modified magnesium hydroxides, 15 parts of zinc borates, 25 parts of Octyl adipates, 10 parts of calcium-zinc composite stabilizing agents, 5 parts of clorafins etc., mixing under the normal temperature, carry out high-speed kneading at 80-110 ℃, drop into again that twin screw extruder is mixing, granulation, the control temperature obtains finished product at 130-180 ℃.
Application Example 2:
(1) raw materials pretreatment: the water intaking magnesite is raw material, obtains the natural brucite ore deposit that content is high, whiteness is good by artificial selection or machine screening, and whiteness is more than 90%, and magnesium hydroxide content is the natural brucite more than 94%; And become 5-10 μ m pellet through the broken crusher machine in Hubei Province;
(2) pulverize modification: in the machinery mill, drop into the broken good pellet 200KG of crusher machine in Hubei Province, start pulverizer, in the spraying measuring apparatus, add 8 KG vinyl cyanide simultaneously, the 8KG maleic anhydride, 0.4 the KG benzoyl peroxide, 30KG acetone stirs, add successively again the 10KG silane coupling agent, the 3KG titanate coupling agent is mixed into solution, sprays in the impact grinding cavity, pouring is on the pellet surface, add in the 20min, make the brucite powder temperature remain on 105 ℃, insulation reaction 60min, then discharging makes in-situ polymerization brucite powder fire retardant.
(3) 65 weight part PVC and 35 parts of EVA blend are even, add 20 parts of superfine modified magnesium hydroxides, 15 parts of zinc borates, 25 parts of Octyl adipates, 10 parts of calcium-zinc composite stabilizing agents, 5 parts of clorafins etc., mixing under the normal temperature, carry out high-speed kneading at 80-110 ℃, drop into again that twin screw extruder is mixing, granulation, the control temperature obtains finished product at 130-180 ℃.
The specific embodiment test result:
| Test event | Unit | Embodiment 1 | Embodiment 2 |
| Breaking tenacity | MPa | 15 | 15 |
| Elongation at break | % | 320 | 310 |
| Smoke density SDR value | ? | 56 | 53 |
| Oxygen index | % | 35 | 35 |
Claims (10)
1. the preparation method of superfine modified brucite flame-retardant agent is characterized in that: this fire retardant adopts the preparation of in-situ polymerization surface treatment method, and each raw materials quality umber is as follows,
100 parts of brucites
Monomer or performed polymer 2-10 part
Initiator 0.02-1 part
Activator 0.5-5 part
Modified additive 0-10 part
Solvent 10-30 part.
2. the preparation method of superfine modified brucite flame-retardant agent according to claim 1, it is characterized in that: the preparation method of this fire retardant is specific as follows,
(a) natural brucite is carried out pre-treatment, comprise screening, drying treatment, and be crushed to 3-5 μ m pellet, and drop in the research of super-pine crush equipment, described research of super-pine crush equipment refers to machinery mill or impact grinding, and powder granularity is at the 1250-2500 order;
(b) monomer or performed polymer, initiator, activator, modified additive are successively packed into according to the above ratio in the spraying measuring apparatus, spray into pellet surface in the ultrafine crusher;
(c) the control temperature of reaction is 60-150 ℃, and the superfine grinding time can prepare the present invention at 20-60min.
3. the preparation method of superfine modified brucite flame-retardant agent according to claim 1, it is characterized in that: described brucite is natural brucite, its magnesium hydroxide content is more than 94%.
4. the preparation method of superfine modified brucite flame-retardant agent according to claim 1, it is characterized in that: described monomer, performed polymer are esters of acrylic acids, co polystyrene type, vinyl cyanide type and maleimide type, tetrafluoroethylene or tetrafluoroethylene/comonomer; Initiator is selected maleic anhydride, peroxycarbonates, ketone peroxide, peroxidation diacyl, the group of organic hydroperoxide and organic peroxy ester.
5. the preparation method of superfine modified brucite flame-retardant agent according to claim 1, it is characterized in that: described activator is selected silicone based, rare earth organism, aluminate coupling agent, titanate coupling agent, acid phosphorous acid ester coupling agent, aluminium/titanium composite coupler, phenolate, inorganic acid salt, sulfonate.
6. the preparation method of superfine modified brucite flame-retardant agent according to claim 1 is characterized in that: described properties-correcting agent is one or more mixing in silicone based, rare earth organism, diphenyl phosphate, triphenylphosphate, di(2-ethylhexyl)phosphate benzene toluene ester, ammonium polyphosphate, phosphoric acid Resorcino diphenyl ester, melamine phosphate, phenyl-phosphonic acid dimethyl ester, dimethyl methyl phosphonate, ammonium pentaborate, sodium metaborate, ammonium borofluoride, barium metaborate, zinc borate and the coating red phosphorus.
7. the preparation method of superfine modified brucite flame-retardant agent according to claim 1, it is characterized in that: described solvent is one or both mixing in acetone, the ethanol etc.
8. the application of the fire retardant of the preparation method of superfine modified brucite flame-retardant agent according to claim 1 and 2 preparation in preparation PVC CABLE MATERIALS.
9. one kind is used superfine modified brucite to be the PVC CABLE MATERIALS of fire retardant, formed by base-material, fire retardant, retardant synergist, softening agent, stablizer, it is characterized in that: described base-material is the mixture of PVC and EVA, described fire retardant is the fire retardant of described employing in-situ polymerization surface treatment method preparation, described retardant synergist is zinc borate, described softening agent is Octyl adipate and UV light absorber, and described stablizer is calcium-zinc composite stabilizing agent.
10. according to claim 9ly a kind ofly use superfine modified brucite to be the PVC CABLE MATERIALS of fire retardant, it is characterized in that: the preparation method, may further comprise the steps: PVC and EVA blend is even, add fire retardant, retardant synergist, softening agent, stablizer, mixing under the normal temperature carries out high-speed kneading at 80-110 ℃, drops into that twin screw extruder is mixing, granulation again, the control temperature obtains this PVC CABLE MATERIALS at 130-180 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105799721A CN103012851A (en) | 2012-12-28 | 2012-12-28 | Preparation method of superfine modified brucite flame retardant and application of superfine modified brucite flame-retardant to PVC (Polyvinyl Chloride) cable material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105799721A CN103012851A (en) | 2012-12-28 | 2012-12-28 | Preparation method of superfine modified brucite flame retardant and application of superfine modified brucite flame-retardant to PVC (Polyvinyl Chloride) cable material |
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| CN103012851A true CN103012851A (en) | 2013-04-03 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107236066A (en) * | 2017-07-10 | 2017-10-10 | 芜湖扬展新材料科技服务有限公司 | The preparation method of polyacrylonitrile composite |
| CN109021363A (en) * | 2018-08-21 | 2018-12-18 | 张玉英 | A kind of polythene material and preparation method of halloysite nanotubes cooperative flame retardant |
| CN114395274A (en) * | 2022-01-12 | 2022-04-26 | 江西广源化工有限责任公司 | Superfine modified magnesium hydroxide, preparation method and application thereof, and flame-retardant polyolefin cable material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891927A (en) * | 2009-09-30 | 2010-11-24 | 如皋市中如化工有限公司 | PVC cable material |
| CN102558913A (en) * | 2011-12-30 | 2012-07-11 | 大连亚泰科技新材料有限公司 | In-situ polymerization surface treatment method in process of refining brucite |
-
2012
- 2012-12-28 CN CN2012105799721A patent/CN103012851A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891927A (en) * | 2009-09-30 | 2010-11-24 | 如皋市中如化工有限公司 | PVC cable material |
| CN102558913A (en) * | 2011-12-30 | 2012-07-11 | 大连亚泰科技新材料有限公司 | In-situ polymerization surface treatment method in process of refining brucite |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107236066A (en) * | 2017-07-10 | 2017-10-10 | 芜湖扬展新材料科技服务有限公司 | The preparation method of polyacrylonitrile composite |
| CN109021363A (en) * | 2018-08-21 | 2018-12-18 | 张玉英 | A kind of polythene material and preparation method of halloysite nanotubes cooperative flame retardant |
| CN109021363B (en) * | 2018-08-21 | 2021-02-02 | 上海方北家居有限公司 | Halloysite nanotube synergistic flame-retardant polyethylene material and preparation method thereof |
| CN114395274A (en) * | 2022-01-12 | 2022-04-26 | 江西广源化工有限责任公司 | Superfine modified magnesium hydroxide, preparation method and application thereof, and flame-retardant polyolefin cable material |
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Application publication date: 20130403 |