CN102558913A - In-situ polymerization surface treatment method in process of refining brucite - Google Patents
In-situ polymerization surface treatment method in process of refining brucite Download PDFInfo
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- CN102558913A CN102558913A CN2011104527636A CN201110452763A CN102558913A CN 102558913 A CN102558913 A CN 102558913A CN 2011104527636 A CN2011104527636 A CN 2011104527636A CN 201110452763 A CN201110452763 A CN 201110452763A CN 102558913 A CN102558913 A CN 102558913A
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Abstract
The invention relates to an in-situ polymerization surface treatment method in the process of refining brucite, and belongs to the field of surface treatment. The method comprises the following steps of: (a) pretreating natural brucite, namely screening, drying, crushing to form granules of 3 to 5 centimeters, and putting into superfine crushing equipment; (b) putting a monomer or a prepolymer, an initiator, an activator, a modified aid and the like into a spray metering device in a ratio, and spraying the mixture to the surfaces of the granules in the superfine crushing equipment; and (c) performing superfine crushing at the reaction temperature of between 60 and 150 DEG C for 20 to 60 minutes to obtain an in-situ polymerization modified brucite powder flame retardant. The in-situ polymerization surface treatment method has the advantage that: technical problems of poor application dispersity and compatibility in materials such as poly ethylene (PE), polypropylene (PP), ethylene (EVA), acrylonitrile butadiene styrene (ABS) and the like are solved; and compared with the conventional treatment method and the conventional modification method, the in-situ polymerization surface treatment method has the advantages that: the additive amount is improved by 10 to 20 percent, and the mechanical property is improved by 20 to 30 percent.
Description
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Technical fieldThe present invention relates to the in-situ polymerization surface treatment method in the brucite thinning process, belong to field of surface treatment.
Background technologyBrucite powder has a good application prospect at aspects such as producing non-halogen flame-retardant cable and other functional high-polymer Halogen, non-toxic material as the flame retardant filler of plastic cement.Because flame retarding efficiency is not high, often need a large amount of fillings (up to more than 150 parts) just can reach flame retardant effect preferably, this moment, the mechanical property of system descended greatly, and this has just influenced its practical application.The conventional process of surface treatment of brucite is a dry method modification, promptly makes superfine powder through superfine grinding equipment, again through height stir machine or continuously activation equipment carry out surface treatment.Main raw material: silane, Triple Pressed Stearic Acid, titanic acid ester, aluminic acid ester etc.; Chinese patent 200610039737.X discloses a kind of surface modifying method and application thereof of natural brucite ultra thin powder; Also be earlier brucite to be carried out fragmentation, grinding, adopting composite coupler is being to carry out activation modification on the surface-treated machine to handle continuously.Domestic existing inorganic combustion inhibitor, this method of most of employing rests on dry mixed, weak effect on the inorganic powder surface treatment technology.Big with external gap on utilisation technology, be mainly reflected in inorganic powder and add the bad dispersibility in the organic synthesis material to, influence the mechanical property of goods.In addition; Chinese patent 95113046.3, Chinese patent 01142497.4, Chinese patent 01111506.8 etc.; The superfine grinding and the surface active modification processing method of brucite are all disclosed; But do not see the relevant situ aggregation method that adopts, in the process that brucite is pulverized, introduce monomer and carry out surface aggregate, in the brucite refinement, carry out superfine grinding and surface activation process.
Summary of the inventionDefective in view of prior art exists the purpose of this invention is to provide the in-situ polymerization surface treatment method in a kind of brucite thinning process, and a kind of new in-situ polymerization modification brucite powder fire retardant especially is provided.
For realizing above-mentioned purpose, the technical solution that the present invention adopted is: the in-situ polymerization surface treatment method in the brucite thinning process is characterized in that: each raw materials quality umber is:
100 parts of brucites
Monomer or performed polymer 2-10 part
Initiator 0.02-1 part
Acvator 0.5-5 part
Modified additive 0-10 part
Solvent is an amount of.
The concrete steps of handling are:
(a) natural brucite is carried out pre-treatment, comprise screening, drying treatment, and be crushed to the 3-5cm pellet, and drop in the superfine grinding equipment.
(b) monomer or performed polymer, initiator, acvator, modified additive etc. are successively packed in the spraying WT-MSR in proportion, spray into pellet surface in the ultrafine crusher.
(c) control reaction temperature 60-150 ℃, the superfine grinding time prepares in-situ polymerization modification brucite powder fire retardant of the present invention at 20-60min.
Said brucite is a natural brucite, is also referred to as brucite, and staple is a Marinco H, and content is more than 94%.
Said superfine grinding equipment is meant machinery mill or impact grinding, and powder granularity can be at the 1250-2500 order.
Said 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 for use, ketone peroxide, peroxo-diacyl, the group of organic hydroperoxide and organic peroxy ester.
That said acvator is selected for use 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, sulphonate.
Said properties-correcting agent is one or more 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.
Said solvent is one or both mixing in acetone, the ethanol etc.
In-situ polymerization surface treatment method in the brucite thinning process; Its beneficial effect is: monomer or performed polymer contain polar group, and shape is vertical coupling keyed jointing structure between powder, and monomer, performed polymer etc. are at the powder surface polymerization reaction take place simultaneously; Form shell-core structure with powder; Be parallel to branch surface spread, the horizontal vertical dual structure makes degree of activation improve greatly, and the surface coats stability and also improves greatly; And shell-nuclear parallel construction makes the surface quite smooth, and powder is highly susceptible to flowing, and has significantly increased the loading level of powder, has solved the technical bottleneck of application decentralization property and consistency difference in materials such as PE, PP, EVA, ABS; Its addition has improved 10-20% than conventional treatment process, and mechanical property improves 20%-30% than conventional method of modifying simultaneously.
Embodiment
Embodiment 1:
(1) raw materials pretreatment: the water intaking magnesite is a raw material, obtains content height, natural brucite ore deposit that whiteness is good through the screening of manual work selection or machine, and whiteness is more than 90%, and Marinco H content is the natural brucite more than 94%; And become the 5-10cm pellet through the broken crusher machine in Hubei Province;
(2) pulverizing modification handles: in impact grinding, drop into the broken good pellet 200KG of crusher machine in Hubei Province, start kibbler, in the spraying WT-MSR, add 12 KG vinylbenzene, 0.5 KG Lucidol simultaneously; 30KG ethanol stirs, and adds the 10KG silane coupling agent more successively; The 3KG triphenylphosphate mixes, and sprays in the impact grinding cavity; Pouring adds in the 15min on the pellet surface, makes the brucite powder temperature remain on 90 ℃; Insulation reaction 40min, discharging then makes in-situ polymerization brucite powder fire retardant.Record degree of activation and can reach 95%, powder granularity reaches 2500 orders.
Above-mentioned 2500 order fire retardant powders are mixed with EVA with 55% ratio, be injection molded into the standard batten, record oxygen index and reach the V1 level, tensile strength can reach 14MPa, and elongation at break can reach 25%.Above-mentioned 2500 order fire retardant powders are mixed with EVA with 65% ratio, be injection molded into the standard batten, record oxygen index and reach the V0 level, tensile strength can reach 18MPa, and elongation at break can reach 35%.
Embodiment 2:
(1) raw materials pretreatment: with embodiment 1;
(2) pulverizing modification handles: in the machinery mill, drop into the broken good pellet 200KG of crusher machine in Hubei Province, start kibbler, in the spraying WT-MSR, add 8 KG vinyl cyanide, the 8KG maleic anhydride simultaneously; 0.4 the KG Lucidol, 30KG acetone stirs, and adds the 5KG silane coupling agent more successively; The 3KG titanate coupling agent, the 3KG zinc borate is mixed into solution, sprays in the impact grinding cavity; Pouring adds in the 20min on the pellet surface, makes the brucite powder temperature remain on 105 ℃; Insulation reaction 60min, discharging then makes in-situ polymerization brucite powder fire retardant.Record degree of activation and can reach 98%, powder granularity reaches 2500 orders.
Above-mentioned 2500 order fire retardant powders are mixed with PP with 55% ratio, be injection molded into the standard batten, record oxygen index and reach the V1 level, tensile strength can reach 20MPa, and elongation at break can reach 33%.Above-mentioned 2500 order fire retardant powders are mixed with PP with 65% ratio, be injection molded into the standard batten, record oxygen index and reach the V0 level, tensile strength can reach 31MPa, and elongation at break can reach 50%.
Claims (7)
1. the in-situ polymerization surface treatment method in the brucite thinning process, it is characterized in that: the concrete steps of processing are:
(a) natural brucite is carried out pre-treatment, comprise screening, drying treatment, and be crushed to the 3-5cm pellet, and drop in the superfine grinding equipment;
(b) monomer or performed polymer, initiator, acvator, modified additive etc. are successively packed in the spraying WT-MSR in proportion, spray into pellet surface in the ultrafine crusher;
(c) control reaction temperature 60-150 ℃, the superfine grinding time prepares in-situ polymerization modification brucite powder fire retardant of the present invention at 20-60min.
2. the in-situ polymerization surface treatment method in the brucite thinning process according to claim 1 is characterized in that: each raw materials quality percentage umber is:
100 parts of brucites
Monomer or performed polymer 2-10 part
Initiator 0.02-1 part
Acvator 0.5-5 part
Modified additive 0-10 part
Solvent is an amount of.
3. the in-situ polymerization surface treatment method in the brucite thinning process according to claim 1 is characterized in that: said superfine grinding equipment is meant machinery mill or impact grinding, and powder granularity can be at the 1250-2500 order.
4. the in-situ polymerization surface treatment method in the brucite thinning process according to claim 1; It is characterized in that: said monomer, performed polymer are esters of acrylic acids; The co polystyrene type, vinyl cyanide type and maleimide type, tetrafluoroethylene or tetrafluoroethylene/comonomer; Initiator is selected maleic anhydride, peroxycarbonates for use, ketone peroxide, peroxo-diacyl, the group of organic hydroperoxide and organic peroxy ester.
5. the in-situ polymerization surface treatment method in the brucite thinning process according to claim 1; It is characterized in that: said acvator is selected silicone based, rare earth organism, aluminate coupling agent, titanate coupling agent, acid phosphorous acid ester coupling agent, aluminium/titanium composite coupler, phenolate for use; Inorganic acid salt, sulphonate.
6. the in-situ polymerization surface treatment method in the brucite thinning process according to claim 1 is characterized in that: said properties-correcting agent is one or more 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 in-situ polymerization surface treatment method in the brucite thinning process according to claim 1 is characterized in that: said solvent is one or both mixing in acetone, the ethanol etc.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103012851A (en) * | 2012-12-28 | 2013-04-03 | 大连亚泰科技新材料股份有限公司 | Preparation method of superfine modified brucite flame retardant and application of superfine modified brucite flame-retardant to PVC (Polyvinyl Chloride) cable material |
| CN104211994A (en) * | 2014-08-21 | 2014-12-17 | 安徽吉安特种线缆制造有限公司 | Modified brucite for low-smoke halogen-free flame-retardant control cable material and preparation method of modified brucite |
| CN104448395A (en) * | 2014-12-04 | 2015-03-25 | 苏州润佳工程塑料股份有限公司 | Composite inorganic mineral powder filler and preparation method thereof |
| CN104479171A (en) * | 2014-12-04 | 2015-04-01 | 苏州润佳工程塑料股份有限公司 | Compound inorganic mineral powder filling material and preparation method thereof |
| CN104662103A (en) * | 2012-09-25 | 2015-05-27 | 芬欧汇川集团 | Method for producing basic products for use as e.g. alkalizing agent (soda lye substitute), for ground stabilization or as filler/pigment |
| CN105236805A (en) * | 2015-09-09 | 2016-01-13 | 武汉源锦商品混凝土有限公司 | Polycarboxylic acid surface modified ultrafine stone powder and preparation method thereof |
| CN107216418A (en) * | 2017-07-10 | 2017-09-29 | 芜湖扬展新材料科技服务有限公司 | The preparation method of Polyacrylate Composites |
| CN108410015A (en) * | 2018-02-09 | 2018-08-17 | 林中 | A kind of special no current mark pearlescent pigment of plastic cement and preparation method thereof |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104662103A (en) * | 2012-09-25 | 2015-05-27 | 芬欧汇川集团 | Method for producing basic products for use as e.g. alkalizing agent (soda lye substitute), for ground stabilization or as filler/pigment |
| CN103012851A (en) * | 2012-12-28 | 2013-04-03 | 大连亚泰科技新材料股份有限公司 | Preparation method of superfine modified brucite flame retardant and application of superfine modified brucite flame-retardant to PVC (Polyvinyl Chloride) cable material |
| CN104211994A (en) * | 2014-08-21 | 2014-12-17 | 安徽吉安特种线缆制造有限公司 | Modified brucite for low-smoke halogen-free flame-retardant control cable material and preparation method of modified brucite |
| CN104448395A (en) * | 2014-12-04 | 2015-03-25 | 苏州润佳工程塑料股份有限公司 | Composite inorganic mineral powder filler and preparation method thereof |
| CN104479171A (en) * | 2014-12-04 | 2015-04-01 | 苏州润佳工程塑料股份有限公司 | Compound inorganic mineral powder filling material and preparation method thereof |
| CN105236805A (en) * | 2015-09-09 | 2016-01-13 | 武汉源锦商品混凝土有限公司 | Polycarboxylic acid surface modified ultrafine stone powder and preparation method thereof |
| CN107216418A (en) * | 2017-07-10 | 2017-09-29 | 芜湖扬展新材料科技服务有限公司 | The preparation method of Polyacrylate Composites |
| CN108410015A (en) * | 2018-02-09 | 2018-08-17 | 林中 | A kind of special no current mark pearlescent pigment of plastic cement and preparation method thereof |
| 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 |
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Application publication date: 20120711 |