CN106243779A - A kind of process that inorganic powder material is carried out organic coating - Google Patents

A kind of process that inorganic powder material is carried out organic coating Download PDF

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Publication number
CN106243779A
CN106243779A CN201610737892.2A CN201610737892A CN106243779A CN 106243779 A CN106243779 A CN 106243779A CN 201610737892 A CN201610737892 A CN 201610737892A CN 106243779 A CN106243779 A CN 106243779A
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powder
spray
organic coating
carried out
powder material
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王强
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WEIFANG DAYAO NEW MATERIAL CO Ltd
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WEIFANG DAYAO NEW MATERIAL CO Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/04—Compounds of zinc
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10—Treatment with macromolecular organic compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/11—Powder tap density
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Polymerisation Methods In General (AREA)

Abstract

The invention discloses a kind of process that inorganic powder material is carried out organic coating, first by small-molecular-weight, high density polyethylene (HDPE) powder, solid oxidizer (KMnO4 KClO4,Na2O2、K2O2), metalloscene catalyst etc. is common adds in oil heating revolving reaction still, then constant speed is heated to a steady temperature maintaining segment time, it is allowed to slowly occur oxidation reaction, prepare OPE, the OPE of preparation is added emulsifying agent, co-emulsifier, deionized water, polymerization inhibitor etc. and makes emulsion, oxidized polyethylene wax emulsion atomization will be made again inorganic powder material will be carried out spray stirring, it is achieved the organic coating to inorganic particle.

Description

A kind of process that inorganic powder material is carried out organic coating
Technical field
The present invention relates to a kind of process that inorganic powder material is carried out organic coating, specifically, be a kind of right Add in magnesium hydrate powder, titanium dioxide, high-purity industrial goods zinc sulphide powder, weight light calcium powder and various inorganic pigment powder body etc. In organic composite material, in order to strengthen inorganic material with the interface binding power of organic material, and inorganic powder surface is had The preparation technology of machine cladding, belongs to chemical technology field.
Background technology
Plastics industry has become one of three big pillar industries of country, adds various inorganic filler and give in plastic resin Plastics possess different specific functions, such as, add hardness and the flame retardant effect of calcium powder energy reinforced plastics, and give product appearance Color；Add the flame retardant effect of the inorganic material energy reinforced plastics product such as magnesium hydroxide, aluminium hydroxide；Long glass fiber reinforced composite wood Material adds zinc sulphide powder and can make the display white of roving glass fiber composite, moreover it is possible to strengthen the intensity of roving glass fiber composite； Various inorganic pigments are also had to give the colourful face of corresponding product during adding the various organic resin such as PE, PP, PET to Color.But macromolecule organic material and inorganic material are in recombination process, there will be interface between the two, this interface binding power Size can to composite produce considerable influence.
Exemplary embodiments: it is widely used lightweight, Materials with High Strength that long glass fiber reinforced heat melts polypropylene (PP) material, is vapour Turner industry substitutes iron and steel, realizes lightweight, the energy-conservation material that is best suitable for, but exists between long glass fibres and PP material and combine Interface, if long glass fibres does not carry out surface process, roving glass fiber heat is melted the intensity of polypropylene material and is not just reached technology and want Ask, and then affect using and selling of product.The same inorganic powder material processed without organic coating is at the organic material of macromole In material presented in aggregate, but owing to particle surface is incompatible with matrix, exist bright between particle agglomeration and matrix Aobvious boundary even produces tiny holes, and during material brittle failure, the granule of inorganic particle is escaped and is easily formed cavity, and does not carries out organic The filling in the base of the inorganic particle of cladding is uneven, affects product quality and outward appearance.
Summary of the invention
The technical problem to be solved in the present invention is for above not enough, it is provided that one carries out organic bag to inorganic powder material The process covered, the inorganic particle prepared based on this kind of technique and organic base material have good combination interface, with organic group Material is firmly combined with, good dispersion in the course of processing, soilless sticking and caking phenomenon.The present invention has that flow process is distinct, controllability is strong Advantage.
In order to solve above technical problem, the technical solution used in the present invention is as follows: inorganic powder material is carried out by one The process of organic coating, it is characterised in that: described process comprises the following steps:
(1) by high density polyethylene (HDPE) powder, solid oxidizer powder, metallocene catalyst, polymerization inhibitor, the same fashionable dress of surfactant Enter in oil reacting by heating still, and be uniformly mixed.
(2) rotate oil reacting by heating still, gradually heat up, programming rate is 1.0 DEG C-2.5 DEG C/min, be warming up to 120 DEG C- It is incubated 72-96 hour, continuous Stirring batch mixing during insulation when 145 DEG C.
(3), after insulation terminates, it is cooled to room temperature and obtains OPE powder.
(4) step (3) is obtained OPE powder, add in pyroreaction still, be simultaneously introduced deionized water, breast The auxiliary agents such as agent, co-emulsifier, initiator, alcohol ether solvent, stabilizer, stirring.
(5) being sealed by reactor, pressurization heats up, and pressure reaches 5.06 × 105～1.013 × 106During Pa, stop pressurization, rise Warm to 110-140 DEG C, temperature retention time 12-36 hour, carry out high-speed stirred during insulation；
(6) insulation terminates, and stops stirring, and decompression cooling down, to room temperature, obtains oxidized polyethylene wax emulsion.
(7) oxidized polyethylene wax emulsion that (6) prepare adding deionized water regulation concentration is 25-45%, adds triethanolamine Regulate the pH of emulsion between 7.5-9.0, load after filtration in spray reactor fluid box.
(8) inorganic powder material is loaded in sealing spray reactor lower layers of containers, then by oxidized polyethylene wax emulsion Atomizing spray is on inorganic particle powder surface, and the most quickly stirring, makes spray emulsion uniform coated powder granule, spray time It is about 10-30 minute.
(9), after spray terminates, continue stirring and continue 6-12 hour, treat that powder surface takes out after drying, reheat and dry 3-5 Hour, period is continuously stirred to prevent heating caking.
(10) drying terminates, cooling, screening, barrelling.
A kind of prioritization scheme, in step (1), solid oxidizer powder is KMnO4 KClO4,Na2O2Or K2O2, purity is for dividing Analysing pure, addition is the 5-15% of polyethylene powder quality；
Further, in step (1), metallocene catalyst addition is the 5-10% of inorganic particle quality, polymerization inhibitor, surface activity Agent addition is the 1.2-3.0% of polyethylene powder quality.
Further, in step (4), deionized water quality is 1-3 times of polyethylene powder quality；
Emulsifying agent is stearic acid sodium, fat alcohol polyethylene ether series, arabic gum, isomery 13 polyoxyethylene ether, benzene sulfonamide One or more in acid sodium compound, and addition is the 15-30% of polyethylene powder quality；
Co-emulsifier is one or more in Oleum Terebinthinae, triethanolamine, butyl glycol ether, polyglycerin ester propylene glycol, n-butyl alcohol Compounding, addition is the 10-25% of polyethylene powder quality.Initiator is potassium peroxydisulfate, sodium peroxydisulfate or Ammonium persulfate. etc., Addition is the 0.5-1.0% of polyethylene quality；
The mass percent concentration of alcohol ether solvent is 45%-60%, addition 50-200L.Stabilizer is calcium stearate, stearic acid Magnesium, zinc stearate or calcium-zinc composite stabilizing agent, addition is the 3-5% of polyethylene quality.
Further, the triethanolamine concentrations adding regulation ph value of emulsion in (7) is 10%.
Further, in step (8), atomizing and oxidizing polythene wax emulsion spray flow rate is 10-60ml/s.
Further, in step (9), spray end post-heating drying temperature is 60-80 DEG C.
The present invention uses above technical scheme, compared with prior art, has the advantage that
(1) present invention process flow process is distinct, relatively low to equipment requirements, energy-conserving and environment-protective, product cut size good dispersion, with organic material The compatibility good, do not produce reunion and thin phenomenon of luming, and add to material does not reduce its mechanical property.
(2) with low-molecular-weight high density polyethylene (HDPE) as raw material, with solid oxidizer powder as oxidant, the oxidation of preparation gathers Ethylene waxes material, non-volatility gas, safety and environmental protection.
(3), in course of reaction, adding emulsion adjuvant is to promote that OPE melts, improving the cloud point of emulsion.
(4) organic coating to inorganic particle uses and seals atomizing spray mode, decreases the consumption of organic coating emulsion, Improve efficiency, reduce cost.
(5) pH of regulation emulsion is between 7.8-9.2, and beneficially emulsion is uniform, stable, breakdown of emulsion does not occur, is layered and ties Block phenomenon, the most actually used and long-term preservation.
(6) surface moisture of product is 0.05%；Specific surface area is 8.76-14.64m2/g；Granularity (D50) is 15-45 μm； Bulk density is 0.85g/m3。
(7) after the inorganic powder material being coated with adds organic substrate to: density 1.50g/cm3；Hot strength 29.2Mpa； Elongation at break 54%；Impact slight 8.31KJ/m2；Hardness 81 Vicat softening point 89.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.But the invention is not restricted to the specific examples being exemplified below. In embodiment, inorganic particle used is high-purity industrial goods zinc sulfide powder, and purity is 97.0%, and particle diameter is (D50) 2-6 μm, white Powder；But it is not limited to high-purity industrial goods zinc sulfide powder.
Embodiment 1, a kind of process that inorganic powder material carries out organic coating, this process includes following step Rapid:
(1) by high density polyethylene (HDPE) powder 100kg, solid oxidizer powder 5kg, metallocene catalyst 5kg, polymerization inhibitor 1.2kg, Surfactant 1.2kg is simultaneously charged in oil reacting by heating still, and is uniformly mixed.
(2) rotating oil reacting by heating still, gradually heat up, programming rate is 1.0 DEG C/min, is warming up to insulation 72 when 110 DEG C Hour, continuous Stirring batch mixing during insulation.
(3), after insulation terminates, it is cooled to room temperature and obtains OPE powder.
(4) step (3) is obtained OPE powder, add in pyroreaction still, be simultaneously introduced deionized water 100L, emulsifying agent 15kg, co-emulsifier 10kg, initiator 0.5kg, alcohol ether solvent 50L, stabilizer 3kg auxiliary agent, stirring.
(5) being sealed by reactor, pressurization heats up, and pressure reaches 5.06 × 105During Pa, stop pressurization, be warming up to 110 DEG C, Temperature retention time 12 hours, carries out high-speed stirred during insulation；
(6) insulation terminates, and stops stirring, and decompression cooling down, to room temperature, obtains oxidized polyethylene wax emulsion.
(7) oxidized polyethylene wax emulsion that (6) prepare adding deionized water regulation concentration is 25%, adds triethanolamine The pH of regulation emulsion, 7.5, loads after filtration in spray reactor fluid box.
(8) inorganic powder material is loaded in spray reactor lower layers of containers, then oxidized polyethylene wax emulsion is atomized Spray is on inorganic particle powder surface, and the most quickly stirring, makes spray emulsion uniform coated powder granule, and spray time is about 10-30 minute.
(9), after spray terminates, continue stirring and continue 6-12 hour, treat that powder surface takes out after drying, reheat and dry 3-5 Hour to dry, period continuously stirred with prevent heating caking.
(10) drying terminates, cooling, screening, barrelling.
Technical specification is as follows:
Process based prediction model Standard
Outward appearance White powder
Surface moisture, % 0.05
Specific surface area, m2/g 16.52
Granularity (D50), μm 35-50
Bulk density, g/m3 0.88
Executing example 2, a kind of process that inorganic powder material carries out organic coating, this process comprises the following steps:
(1) by high density polyethylene (HDPE) powder 100kg, solid oxidizer powder 8kg, metallocene catalyst 8kg, polymerization inhibitor 1.5kg, Surfactant 1.5kg is simultaneously charged in oil reacting by heating still, and is uniformly mixed.
(2) rotating oil reacting by heating still, gradually heat up, programming rate is 1.5 DEG C/min, is warming up to insulation 76 when 115 DEG C Hour, continuous Stirring batch mixing during insulation.
(3), after insulation terminates, it is cooled to room temperature and obtains OPE powder.
(4) step (3) is obtained OPE powder, add in pyroreaction still, be simultaneously introduced deionized water 100L, emulsifying agent 18kg, co-emulsifier 15kg, initiator 0.6kg, alcohol ether solvent 80L, stabilizer 3.5kg auxiliary agent, stirring.
(5) being sealed by reactor, pressurization heats up, and pressure reaches 7.12 × 105During Pa, stop pressurization, be warming up to 110 DEG C, Temperature retention time 15 hours, carries out high-speed stirred during insulation；
(6) insulation terminates, and stops stirring, and decompression cooling down, to room temperature, obtains oxidized polyethylene wax emulsion.
(7) oxidized polyethylene wax emulsion that (6) prepare adding deionized water regulation concentration is 29%, adds triethanolamine The pH of regulation emulsion, 7.9, loads after filtration in spray reactor fluid box.
(8) inorganic powder material is loaded in spray reactor lower layers of containers, then oxidized polyethylene wax emulsion is atomized Spray is on inorganic particle powder surface, and the most quickly stirring, makes spray emulsion uniform coated powder granule, and spray time is about 10-30 minute.
(9), after spray terminates, continue stirring and continue 6-12 hour, treat that powder surface takes out after drying, reheat and dry 3-5 Hour to dry, period continuously stirred with prevent heating caking.
(10) drying terminates, cooling, screening, barrelling.
Technical specification is as follows:
Process based prediction model Standard
Outward appearance White powder
Surface moisture, % 0.05
Specific surface area, m2/g 14.64
Granularity (D50), μm 30-45
Bulk density, g/m3 0.85
Embodiment 3, a kind of process that inorganic powder material is carried out organic coating, this process comprises the following steps:
(1) by high density polyethylene (HDPE) powder 100kg, solid oxidizer powder 10kg, metallocene catalyst 9kg, polymerization inhibitor 1.8kg, surfactant 1.8kg are simultaneously charged in oil reacting by heating still, and are uniformly mixed.
(2) rotating oil reacting by heating still, gradually heat up, programming rate is 1.8 DEG C/min, is warming up to insulation 82 when 120 DEG C Hour, continuous Stirring batch mixing during insulation.
(3), after insulation terminates, it is cooled to room temperature and obtains OPE powder.
(4) step (3) is obtained OPE powder, add in pyroreaction still, be simultaneously introduced deionized water 100L, emulsifying agent 20kg, co-emulsifier 18kg, initiator 0.7kg, alcohol ether solvent 100L, stabilizer 4.0kg auxiliary agent, stirring.
(5) being sealed by reactor, pressurization heats up, and pressure reaches 7.58 × 105During Pa, stop pressurization, be warming up to 110 DEG C, Temperature retention time 18 hours, carries out high-speed stirred during insulation；
(6) insulation terminates, and stops stirring, and decompression cooling down, to room temperature, obtains oxidized polyethylene wax emulsion.
(7) oxidized polyethylene wax emulsion that (6) prepare adding deionized water regulation concentration is 25-45%, adds triethanolamine Regulate the pH of emulsion 8.4, load after filtration in spray reactor fluid box.
(8) inorganic powder material is loaded in spray reactor lower layers of containers, then oxidized polyethylene wax emulsion is atomized Spray is on inorganic particle powder surface, and the most quickly stirring, makes spray emulsion uniform coated powder granule, and spray time is about 10-30 minute.
(9), after spray terminates, continue stirring and continue 6-12 hour, treat that powder surface takes out after drying, reheat and dry 3-5 Hour to dry, period continuously stirred with prevent heating caking.
(10) drying terminates, cooling, screening, barrelling.
Technical specification is as follows:
Process based prediction model Standard
Outward appearance White powder
Surface moisture, % 0.05
Specific surface area, m2/g 11.33
Granularity (D50), μm 20-30
Bulk density, g/m3 0.85
Embodiment 4, a kind of process that inorganic powder material is carried out organic coating, this process comprises the following steps:
(1) by high density polyethylene (HDPE) powder 100kg, solid oxidizer powder 15kg, metallocene catalyst 10kg, polymerization inhibitor 2.0kg, surfactant 2.0kg are simultaneously charged in oil reacting by heating still, and are uniformly mixed.
(2) rotating oil reacting by heating still, gradually heat up, programming rate is 2.0 DEG C/min, is warming up to insulation 89 when 125 DEG C Hour, continuous Stirring batch mixing during insulation.
(3), after insulation terminates, it is cooled to room temperature and obtains OPE powder.
(4) step (3) is obtained OPE powder, add in pyroreaction still, be simultaneously introduced deionized water 100L, emulsifying agent 25kg, co-emulsifier 20kg, initiator 0.8kg, alcohol ether solvent 150L, stabilizer 4.5kg auxiliary agent, stirring.
(5) being sealed by reactor, pressurization heats up, and pressure reaches 8.78 × 105During Pa, stop pressurization, be warming up to 110 DEG C, Temperature retention time 18 hours, carries out high-speed stirred during insulation；
(6) insulation terminates, and stops stirring, and decompression cooling down, to room temperature, obtains oxidized polyethylene wax emulsion.
(7) oxidized polyethylene wax emulsion that (6) prepare adding deionized water regulation concentration is 25-45%, adds triethanolamine Regulate the pH of emulsion 8.7, load after filtration in spray reactor fluid box.
(8) inorganic powder material is loaded in spray reactor lower layers of containers, then oxidized polyethylene wax emulsion is atomized Spray is on inorganic particle powder surface, and the most quickly stirring, makes spray emulsion uniform coated powder granule, and spray time is about 10-30 minute.
(9), after spray terminates, continue stirring and continue 6-12 hour, treat that powder surface takes out after drying, reheat and dry 3-5 Hour to dry, period continuously stirred with prevent heating caking.
(10) drying terminates, cooling, screening, barrelling.
Technical specification is as follows:
Process based prediction model Standard
Outward appearance White powder
Surface moisture, % 0.05
Specific surface area, m2/g 8.76
Granularity (D50), μm 15-25
Bulk density, g/m3 0.85
Embodiment 5, a kind of process that inorganic powder material is carried out organic coating, this process comprises the following steps:
(1) by high density polyethylene (HDPE) powder 100kg, solid oxidizer powder 15kg, metallocene catalyst 10kg, polymerization inhibitor 3.0kg, surfactant 3.0kg are simultaneously charged in oil reacting by heating still, and are uniformly mixed.
(2) rotating oil reacting by heating still, gradually heat up, programming rate is 2.5 DEG C/min, is warming up to insulation 96 when 130 DEG C Hour, continuous Stirring batch mixing during insulation.
(3), after insulation terminates, it is cooled to room temperature and obtains OPE powder.
(4) step (3) is obtained OPE powder, add in pyroreaction still, be simultaneously introduced deionized water 100L, emulsifying agent 30kg, co-emulsifier 25kg, initiator 1.0kg, alcohol ether solvent 150L, stabilizer 5.0kg, stirring.
(5) being sealed by reactor, pressurization heats up, and when pressure reaches 5.06 × 105～1.013 × 106Pa, stops pressurization, It is warming up to 110 DEG C, temperature retention time 18 hours, carry out high-speed stirred during insulation；
(6) insulation terminates, and stops stirring, and decompression cooling down, to room temperature, obtains oxidized polyethylene wax emulsion.
(7) oxidized polyethylene wax emulsion that (6) prepare adding deionized water regulation concentration is 25-45%, adds triethanolamine Regulate the pH of emulsion between 7.5-9.0, load after filtration in spray reactor fluid box.
(8) inorganic powder material is loaded in spray reactor lower layers of containers, then oxidized polyethylene wax emulsion is atomized Spray is on inorganic particle powder surface, and the most quickly stirring, makes spray emulsion uniform coated powder granule, and spray time is about 10-30 minute.
(9), after spray terminates, continue stirring and continue 6-12 hour, treat that powder surface takes out after drying, reheat and dry 3-5 Hour to dry, period continuously stirred with prevent heating caking.
(10) drying terminates, cooling, screening, barrelling.
Technical specification is as follows:
Process based prediction model Standard
Outward appearance White powder
Surface moisture, % 0.05
Specific surface area, m2/g 8.76
Granularity (D50), μm 18-25
Bulk density, g/m3 0.85
The raw material related in above example is commercially available prod in the market, unless specifically stated otherwise, involved Percentage ratio be mass percent.
The above is the citing of the specific embodiment of the invention, and it is common that the part addressed the most in detail is this area The common knowledge of technical staff.
More than implement in embodiment the manufacturer of catalyst, polymerization inhibitor and surfactant and product without any special Requirement, domestic more manufacturer produces.
Metallocene catalyst provide producer have: FOX graceful science and technology (Beijing) company limited, Hangzhou marine origin Chemical Co., Ltd., Shanghai cyclopentadienyl chemical reagent company limited, prosperous Science and Technology Ltd. of Beijing state side, Langfang Hao Ke development in science and technology company limited, orchid Zhou Tenghua Chemical Industry Science Co., Ltd etc. is all provided with.
Polymerization inhibitor provides producer: the upper easy Chemical Co., Ltd. of sea light, Changzhou Yu Rong Chemical Co., Ltd., Henan perseverance association Heavy chemicals sell company limited, Rui Kai trade Co., Ltd of Zhuhai City, Hangzhou Zhuo Jing Chemical Co., Ltd., the happy nation in Changzhou be combined Materials Co., Ltd, Qingdao Jie get Jia new material Science and Technology Ltd., Dongguan City Long Hai new material Science and Technology Ltd. etc..
Surfactant provides producer: Shanghai Xue Jie Chemical Co., Ltd., Shanghai Jinshan longitude and latitude Chemical Co., Ltd., Shanghai The domestic more manufacturing enterprises such as Su Ke Chemical Co., Ltd., Zibo Hai Jie Chemical Co., Ltd..
Test:
1, main raw material(s):
The most uncoated high-purity industrial goods zinc sulphide powder (97%): by our company commercially available prod；
(2) high-purity industrial goods zinc sulphide powder after cladding, the product of embodiment 5 preparation,
(3) PVC raw material (powder), is provided by photoelectron plastic cement company limited of Weifang China.
2, checking flow process
(1) without any interpolation PVC melted injection member, numbered 1# sample；
(2) add uncoated high-purity industrial goods zinc sulphide powder PVC powder melted injection member, numbered 2# sample；
(3) add organic coating high-purity industrial goods zinc sulphide powder PVC melted injection member, numbered 3# sample；
After inorganic particle is mixed homogeneously with PVC powder, appropriate stabilizer, load in injection molding machine of plastic, be molded into motor vehicles and join Part, carries out coherent detection test.
3, result and discussion
Technical specification detects such as following table:
Note: uncoated high-purity industrial goods zinc sulphide powder, be coated with high-purity industrial goods zinc sulphide powder addition and be all the 10% of PVC mass.
By above technical specification it can be seen that coated inorganic powder material adds under organic substrate after-drawing intensity Fall change is little, and elongation at break has had obvious growth, product cut size good dispersion, and the compatibility with organic material is good, no Producing and reunite and thin phenomenon of luming, the mechanics mechanical performance added in organic material relative to uncoated inorganic powder has had bright Aobvious improves.
Through analyzing:
Addition emulsion adjuvant promotes OPE and melts, and improves the cloud point of emulsion.
Use and seal atomizing spray mode, decrease the consumption of organic coating emulsion, improve efficiency, reduce cost.
The pH of emulsion is between 7.8-9.2, and emulsion is uniform, stable, and breakdown of emulsion, layering and caking phenomenon do not occur, and is beneficial to real Border uses and long-term preservation.
Illustrate to process and can be obviously improved inorganic powder material and organic material by inorganic powder material carries out organic coating The fusion of material connects, and improves the integrated application performance of composite.
Above-mentioned detailed description of the invention is exemplary, is to enable those skilled in the art to be better understood from this Summary of the invention, should not be understood as limiting the scope of the invention, as long as according to changing that technical solution of the present invention is made Enter, each fall within protection scope of the present invention, the part addressed the most in detail be those of ordinary skill in the art known often Know.

Claims (7)

1. the process that inorganic powder material is carried out organic coating, it is characterised in that: described process include with Lower step:
(1) by high density polyethylene (HDPE) powder, solid oxidizer powder, metallocene catalyst, polymerization inhibitor, the same fashionable dress of surfactant Enter in oil reacting by heating still, and be uniformly mixed；
(2) rotating oil reacting by heating still, gradually heat up, programming rate is 1.0 DEG C-2.5 DEG C/min, is warming up to 120 DEG C-145 DEG C Shi Baowen 72-96 hour, continuous Stirring batch mixing during insulation；
(3), after insulation terminates, it is cooled to room temperature and obtains OPE powder；
(4) step (3) is obtained OPE powder, add in pyroreaction still, be simultaneously introduced deionized water, emulsifying The auxiliary agents such as agent, co-emulsifier, initiator, alcohol ether solvent, stabilizer, stirring；
(5) being sealed by reactor, pressurization heats up, and pressure reaches 5.06 × 105～1.013 × 106During Pa, stop pressurization, be warming up to 110-140 DEG C, temperature retention time 12-36 hour, carry out high-speed stirred during insulation；
(6) insulation terminates, and stops stirring, and decompression cooling down, to room temperature, obtains oxidized polyethylene wax emulsion；
(7) oxidized polyethylene wax emulsion that (6) prepare adding deionized water regulation concentration is 25-45%, adds triethanolamine and adjusts The pH of joint emulsion, between 7.5-9.0, loads after filtration in spray reactor fluid box；
(8) inorganic powder material is loaded in sealing spray reactor lower layers of containers, then oxidized polyethylene wax emulsion is atomized Spray is on inorganic particle powder surface, and the most quickly stirring, makes spray emulsion uniform coated powder granule, and spray time is about 10-30 minute；
(9) after spray terminates, continuing stirring and continue 6-12 hour, treat that powder surface takes out after drying, it is little that reheating dries 3-5 Time, period is continuously stirred to prevent heating caking；
(10) drying terminates, cooling, screening, barrelling.
A kind of process that inorganic powder material is carried out organic coating the most according to claim 1, it is characterised in that: In step (1), solid oxidizer powder is KMnO4 KClO4,Na2O2Or K2O2, purity is analytical pure, and addition is polyethylene powder The 5-15% of material quality.
A kind of process that inorganic powder material is carried out organic coating the most according to claim 1, it is characterised in that: In step (1), metallocene catalyst addition is the 5-10% of inorganic particle quality, and polymerization inhibitor, surfactant addition are poly- The 1.2-3.0% of ethylene opaque amount.
A kind of process that inorganic powder material is carried out organic coating the most according to claim 1, it is characterised in that: In step (4), deionized water quality is 1-3 times of polyethylene powder quality；
Emulsifying agent is stearic acid sodium, fat alcohol polyethylene ether series, arabic gum, isomery 13 polyoxyethylene ether, benzene sulfonamide One or more in acid sodium compound, and addition is the 15-30% of polyethylene powder quality；
Co-emulsifier is one or more in Oleum Terebinthinae, triethanolamine, butyl glycol ether, polyglycerin ester propylene glycol, n-butyl alcohol Compounding, addition is the 10-25% of polyethylene powder quality；
Initiator is potassium peroxydisulfate, sodium peroxydisulfate or Ammonium persulfate. etc., and addition is the 0.5-1.0% of polyethylene quality；
The mass percent concentration of alcohol ether solvent is 45%-60%, addition 50-200L；
Stabilizer is calcium stearate, magnesium stearate, zinc stearate or calcium-zinc composite stabilizing agent, and addition is the 3-of polyethylene quality 5%。
A kind of process that inorganic powder material is carried out organic coating the most according to claim 1, it is characterised in that: (7) triethanolamine concentrations adding regulation ph value of emulsion in is 10%.
A kind of process that inorganic powder material is carried out organic coating the most according to claim 1, it is characterised in that: In step (8), atomizing and oxidizing polythene wax emulsion spray flow rate is 10-60ml/s.
A kind of process that inorganic powder material is carried out organic coating the most according to claim 1, it is characterised in that: In step (9), spray end post-heating drying temperature is 60-80 DEG C.
CN201610737892.2A 2016-08-29 2016-08-29 A kind of process that inorganic powder material is carried out organic coating Pending CN106243779A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102276904A (en) * 2011-08-19 2011-12-14 龙口市易久化工科技有限公司 Wax emulsion for modifying delustering agent and other inorganic powder materials and preparation method thereof
CN103396563A (en) * 2013-07-04 2013-11-20 潍坊科澜新材料有限公司 Technology for preparing organic cladding emulsion for inorganic powder material
CN103965657A (en) * 2014-05-05 2014-08-06 潍坊大耀新材料有限公司 Surface modification method of ZnS powder
CN104448935A (en) * 2013-09-15 2015-03-25 李志刚 Preparation method for nano-calcium carbonate composite particle

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102276904A (en) * 2011-08-19 2011-12-14 龙口市易久化工科技有限公司 Wax emulsion for modifying delustering agent and other inorganic powder materials and preparation method thereof
CN103396563A (en) * 2013-07-04 2013-11-20 潍坊科澜新材料有限公司 Technology for preparing organic cladding emulsion for inorganic powder material
CN104448935A (en) * 2013-09-15 2015-03-25 李志刚 Preparation method for nano-calcium carbonate composite particle
CN103965657A (en) * 2014-05-05 2014-08-06 潍坊大耀新材料有限公司 Surface modification method of ZnS powder

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Application publication date: 20161221