CN103374194A - Gas phase nano silicon dioxide master batches for plastic modification and preparation method thereof - Google Patents
Gas phase nano silicon dioxide master batches for plastic modification and preparation method thereof Download PDFInfo
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- CN103374194A CN103374194A CN2012101106061A CN201210110606A CN103374194A CN 103374194 A CN103374194 A CN 103374194A CN 2012101106061 A CN2012101106061 A CN 2012101106061A CN 201210110606 A CN201210110606 A CN 201210110606A CN 103374194 A CN103374194 A CN 103374194A
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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
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Abstract
The invention discloses gas phase nano silicon dioxide master batches for plastic modification and a preparation method thereof. The preparation method is characterized by comprising the following steps of: firstly, preparing gas phase method nano silicon dioxide, and performing surface treatment on the nano silicon dioxide by using octamethylcy-clotetrasiloxane of which accounts for 1-10% of the total weight as a treatment agent to ensure that the nano silicon dioxide becomes hydrophobic from being hydrophilic; then slowly stirring and mixing the hydrophobic silicon dioxide with polyethylene which is grafted with maleic anhydride according to the following raw material formula in percentage by weight: 40-60% of grafted polyethylene resin, 60-40% of the hydrophobic silicon dioxide, 0.2-0.6% of an antioxidant and 0.5-1.5% of a dispersant; and finally, extruding the mixed material from a twin-screw extruder for granulating so as to prepare the nano silicon dioxide master batches for plastic modification. The gas phase nano silicon dioxide master batches can be widely used in the industries and fields including plastics, rubbers, daily chemical industry and the like, and the strength, wear resistance, corrosion resistance, lubricating property and the like of a product are significantly improved.
Description
Technical field
The present invention relates to nano-powder material preparation and application thereof.Be specifically related to a kind of modifying plastics gas phase nano silicon-dioxide master batch and preparation method thereof.This master batch can be used for industry and the fields such as plastics, rubber, agricultural chemical, daily-use chemical industry goods, papermaking filler, ink powder filler.Be applied to especially the modifying plastics field, its surface abrasion resistance of the matrix material after its modification, intensity and other each side mechanical property can both be greatly improved.And because product is the form with master batch, in application process, can reach easy to use, environmental friendliness.
Background technology
Silicon is second largest element on the earth, and content is only second to oxygen, and mostly the form with silicon-dioxide exists, and its Application Areas is very extensive.
The traditional production method of silicon-dioxide is roughly the precipitator method, and the precipitator method are again the water glass acidization, adopts water glass solution and acid-respons, obtains through precipitation, filtration, washing, drying and calcining.Reaction formula is: Na2SiO3+2H+-SiO2+2Na++H20.Most domestic manufacturing enterprise adopts the precipitator method.The precipitator method can be divided into traditional precipitator method and special precipitation again, the former refers to the silicon-dioxide of the production take sulfuric acid, hydrochloric acid, CO2 and water glass as basic raw material, and the latter refers to adopt the silicon-dioxide of the special methods productions such as high-gravity technology, sol-gel method, chemical crystal method, secondary crystal method or reversed phase micelle microemulsion method.The silicon-dioxide of producing in this way, particle diameter is large, and purity is low, can only be applied in the low-end product as common material, as natural rubber and elastomeric strengthening agent, toothpaste abrasives etc.
And advanced producer rule is vapor phase process, is called chemical vapour deposition (CAV) method, claims again pyrolysis method, dry method or combustion method.Its raw material is generally silicon tetrachloride, oxygen (or air) and hydrogen, and reaction forms under the high temperature.Reaction formula is: SiCl4+ 2H2+ O2-SiO2+4HCl.Air and hydrogen respectively through pressurization, separate, send into synthetic hydrolysis stove after the cooled dehydrated, silica dehydrator, dust removal and filtration.After the silicon tetrachloride raw material delivered to rectifying tower rectifying, heating evaporation in vaporizer, and take dry, air after filtering as carrier, deliver to synthetic hydrolysis stove.Silicon tetrachloride at high temperature gasifies after (1000 ~ 1800 ℃ of flame temperatures), carries out vapor phase hydrolysis with a certain amount of hydrogen and oxygen (or air) under the high temperature about 1800 ℃; The aerosil particle that generate this moment is superfine, forms aerosol with gas, is difficult for capturing, so make it in collector, be gathered into first larger particles, then collecting through cyclonic separator, send into deacidification furnace again, is 4～6 to be finished product with nitrogenous air blowing aerosil to pH value.
Fumed silica is that silicon-dioxide primary partical that halogenide by silicon forms in hydrolysis under 1000 ℃ or higher temperature, the combustion processes in oxyhydrogen flame mutually collides and forms offspring and form long-chain and the ultramicro powder with surface hydroxyl and planar water that generates.Fumed silica is magical nano material.Because it has uncommon material characteristic, it is minimum particle diameter (particle diameter of primary structure is 7 ~ 40 nanometers), (it is 100 ~ 400m2/g) that the BET method detects to specific surface area greatly, its chaining tendency of very high purity (dioxide-containing silica is not less than 99.8%), make it have the unusual performances such as remarkable reinforcement, thickening property, thixotropy, extinction, dispersiveness, insulativity, non-stick property, benefit is called " industrial monosodium glutamate ".Fumed silica and modified product thereof are widely used in the fields such as plastics, rubber, coating, medicine, tackiness agent, printing ink, makeup, space flight, building, food sanitation agricultural chemicals.It is one of extremely important ultra tiny New Inorganic Materials.Although the particle diameter of fumed silica is little, specific surface area is large, the tensile strength of filling and vulcanization glue, tear strength and wear resistance are all higher; But the consistency of it and hydrocarbon rubbers is relatively poor, and the viscosity of a large amount of filler gums is larger, and processing characteristics is variation with the prolongation of period of storage, and there is sclerosis in sizing material, extrudes the problems such as difficulty and moulding viscosity is poor after storing.This is because the acidity that activated silica hydroxyl, planar water and the preparation technology that the fumed silica surface exists causes its surface to occur, make fumed silica be wetting ability, in organic phase, be difficult to infiltrate and disperse, reduced sulfuration efficient and reinforcing property from face, made it have the field of particular requirement to use at some.Such as, because the specific surface area of high reinforcement fumed silica surpasses 100m2/g, and contain a large amount of Si-OH bases on the surface, so interparticle cohesive force is quite strong, in rubber, be difficult to disperse, very unfavorable to reinforcement; And the Si-OH base is gone back easily and Si-O key or Si-OH effect in the rubber molecule, produces the structurizing phenomenon, brings problem for storage, processing and the application of sizing material.Fumed silica after the modification can effectively reduce Si-OH, and is transformed into hydrophobic surface by hydrophilic surface, thus reach hold concurrently to improve fumed silica in rubber dispersiveness (wetting property) and reduce or avoid the purpose of sizing material recurring structure.Improve its dispersiveness and consistency in organic phase, thereby greatly widened the Application Areas of product, improved the added value of fumed silica.
Infrared spectroscopic study shows, a certain amount of activity hydroxy is contained on the fumed silica surface, the main Types of hydroxyl has: two hydroxyls, isolation hydroxyl and adjacent hydroxyl, different hydroxyls has different reactive behavioies, the existence at hydroxyl activity center makes it have reinforcing property, provides reactive functionality for its surface modification simultaneously.X-ray diffraction pattern proves, the fumed silica one-piece construction is amorphous state, molecule is intensive and degree is higher, particle is tiny (nano level), specific surface area is large, when the temperature below fusing point is heat-treated, though the internal structure of being heated for a long time can not change yet, the oxidation of tetravalence Siliciumatom minor structure unit mainly presents the ternary three dimensional structure in the preparation process in addition.So-called modification fumed silica, react by the certain chemical substance of certain technology utilization and the surface hydroxyl of fumed silica exactly, the amount of elimination or minimizing surface silanol group makes silicon-dioxide become hydrophobicity by wetting ability, to improve it with the affinity of polymeric compositions.The silica sphere modification had both required to remove or reduce the amount of its surface hydroxyl, did not change again its fundamental character.According to the difference of properties-correcting agent, chemical modification method commonly used has following several.Dehydration when the silica sphere hydroxyl is heated to 750 ℃ is at the Surface Creation siloxanes, again with the active polystyrene grafting.The technique of modification: the specific surface area of fumed silica is very large, can not cover simply or be adsorbed on its surface by organism and not improve oilness and dispersiveness.External modified technique commonly used has: the steaming process (often being called dry method) that dry fumed silica contacts with organic steam and reacts; Fumed silica heats the circumfluence method (often being called wet method) that makes the properties-correcting agent boiling reflux with properties-correcting agent; In autoclave, carry out the hydrothermal reaction method of high-temperature high-voltage reaction etc.The early stage study on the modification of adopts wet method more, but the development along with the ultramicro particle fluidization technology, the operation control of fluidized-bed reactor has obtained more successful experience, can reach equally the material contact condition of wet method with dry method, and the dry method modification device can directly be connected in before the device for producing silicon dioxide by adopting vapor deacidification process not only economy but also practicality.By contrast, the solvent that wet method adopts such as benzene, toluene etc. are toxic substances, product separation, purification difficult, and cost is high, seriously polluted.The silicon-dioxide of modification has almost been inherited all high-performances of common fumed silica, and owing to its special hydrophobicity, Application Areas is greatly expanded again.In numerous hydrophobic products, water drain silica with the dimethyldichlorosilane(DMCS) modification is most widely used, it has the tendency that prevents material caking, improve the characteristics such as powder material flowability, can be used for the fields such as synthetic resin moulding compound, fire-fighting fire extinguishing powder, superoxide, after shave powder, powder coating, to improve product processibility, applicability and storage characteristics. adopts different properties-correcting agent and specific technique, can produce the hydrophobic type silica product of a series of various trades mark. only has the enterprise in a few countries such as the U.S., Germany, Japan, the C.I.S., China and area can produce fumed silica and modified product thereof at present in the world, and its heavy industrialization technology is also mended department's monopolization in several large minute such as Degussa, Cabot.Whole world fumed silica overall throughput is about annual 120000 tons, and wherein modified product accounts for 20% of total amount. China fumed silica modification technology is relatively backward, can only small-scale production, and second-rate, therefore base end in the market of present Chinese modification fumed silica is upper is captured by the product of the companies such as Degussa, Cabot, Waker. modification fumed silica price is different and different with the trade mark, is generally 12～250,000 yuan/t.The fumed silica product of exploitation surface modification has good economic and social benefit.
Above-mentioned fumed silica product owing to be that form with powder exists, is often easily reunited, and in use, is added on and is not easy in the different materials to disperse, and dust pollution is arranged, and environment is had a great impact.Particularly the modifying plastics field is used and has been subject to certain restriction.Therefore being prepared into the master batch form has more using value.
Summary of the invention
The objective of the invention is to overcome the deficiency that exists in prior art and the product application, a kind of novel fumed nano silicon-dioxide master batch product with special purpose is provided.
Another object of the present invention provides the preparation method that above-mentioned modifying plastics is used fumed nano silicon-dioxide master batch.
For achieving the above object, the technical solution used in the present invention is:
1. preparing nano silicon dioxide by vapor phase process.
Reaction formula is: SiCl4+ 2H2+ O2-SiO2+4HCl
With the fumed silica of aforesaid method preparation, the particle diameter 7-40 nanometer of its primary particle, the large 50-380 ㎡/g of specific surface area, purity SiO2＞99.8%, general apparent density 50g/l.
2. surface modification treatment
With above-mentioned fumed nano silicon-dioxide, add octamethylcyclotetrasiloxane, in homogenizer, react, chemical modification occurs, become the hydrophobicity product.
Treatment process, flow process are:
(1) component substance
Fumed nano silicon-dioxide 90-99%
Octamethylcyclotetrasiloxane 1-10%
(2) treatment process: above-mentioned component substance is sneaked in the homogenizer, and Temperature Setting is at 120-150 ℃, and speed setting is at 1000-1500 rev/min, churning time 10-20 minute.Namely obtain the special-purpose hydrophobic fumed nano silicon of modifying plastics.
3, master batch preparation
With the silicon-dioxide of above-mentioned processing, carry out low rate mixing with grafted polyethylene (g-PP), oxidation inhibitor (1010/168), dispersion agent (EBS/TAF) and mix, through the melting of twin-screw extrusion unit, mixing, extrude, granulation forms.
Preparation technology, flow process are:
(1) component substance
Maleic anhydride grafted polyethylene 40-60%
Surface-treated nano silicon 60-40%
Antioxidant 1010 0.1-0.3%
Irgasfos 168 0.1-0.3%
Dispersion agent (EBS/TAF) 0.5-1.5%
Above-mentioned EBS/TAF is ethylene bis stearic acid amide
/The modification ethylene bis stearic acid amide.
(2) granulation process
Melt extrude granulation: above-mentioned compound was stirred 10-15 minute at low rate mixing machine (100-150 rev/min); add in the twin screw extruder; the adjusting engine speed is 180 ~ 350rpm; the feeding rotating speed is 250 ~ 800rpm; melt extrude temperature in 160 ~ 250 ℃ of scopes; under the conveying and shearing action of twin screw extruder; fully fusion plastification, mediate mixing; water ring pelletizing or cold drawn bar pelletizing after head is extruded, dry rear packing namely gets modifying plastics fumed nano silicon-dioxide master batch
The technology of the present invention principle is as follows:
The present invention at first uses the standby fumed nano silicon-dioxide of chemical vapour deposition (CAV) legal system, obtains that particle diameter is little, specific surface area is large, purity is high, the nano silicon of high dispersing.The product particle surface of this moment exists siloxanes and silanol, belongs to the wetting ability product, directly uses and receives very large restriction.
Therefore, the present invention processes its surface exactly, mainly is to add octamethylcyclotetrasiloxane, under the certain temperature condition, carry out the high-speed stirring combination treatment, so that chemical modification occurs for siloxanes and silanol and silane and silazane reaction, become hydrophobicity (lipophilic) product.Because the said products is to exist with the powder form, and is not too convenient in storage, accumulating, use etc., has dust floating, affects environment.
On this basis, the present invention mixes the nano silicon of above-mentioned processing and grafted polyethylene and oxidation inhibitor, dispersion agent again, and through the twin screw extruder melting mixing, extruding pelletization makes fumed nano silicon-dioxide master batch.This master batch is by twice dispersing, and the modifying plastics field that is applied to that can be convenient has enlarged its range of application.
Products characteristics of the present invention:
In plastics and coating, improve the intensity of material, the thickening of optimum dispersiveness and rheological polar liquid during wear resistance and scratch resistance processing are used, such as the high addition of the reinforcement of Resins, epoxy silicone elastomer, such as hydrophobicity good in pressing, improve preservative property and improve dielectric properties, such as powder glidant in the cable mixture, such as, environmental friendliness convenient in use procedure in fire-fighting medium.
Description of drawings
Accompanying drawing 1 is process flow sheet of the present invention.
Embodiment
Referring to shown in Figure 1, the preparation method is as follows:
(1) preparation fumed nano silicon-dioxide
(2) above-mentioned nano silicon is carried out surface modification treatment with octamethylcyclotetrasiloxane, make it become hydrophobicity by wetting ability.
(3) mix: grafted polyethylene resin, nano silicon, oxidation inhibitor, dispersion agent are mixed the forcing machine hopper with the low rate mixing machine.
(4) melt extrude granulation: above-mentioned compound is added in the twin screw extruder; the adjusting engine speed is 180 ~ 350rpm; the feeding rotating speed is 250 ~ 800rpm; melt extrude temperature in 160 ~ 250 ℃ of scopes; under the conveying and shearing action of twin screw extruder; fully fusion plastification, mediate mixing, water ring pelletizing or cold drawn bar pelletizing after head is extruded, dry after packing namely get modifying plastics nano silicon master batch.
According to above-mentioned preparation method (hydrophobic fumed silica preparation and surface treatment method thereof are identical, all are that the octamethylcyclotetrasiloxane with gross weight 5% deals with agent):
Embodiment 1
Modifying plastics nano silicon formula of master batch (weight percentage)
(1) grafted polyethylene resin---40%;
(2) hydrophobic fumed nano silicon---60%;
(3) dispersion agent (TAF)----1%
(4) 1010/168 oxidation inhibitor---0.2/0.2%.
This master batch is used for modifying plastics, and addition is 8% to get final product.
Embodiment 2
Modifying plastics nano silicon formula of master batch (weight percentage)
(1) grafted polyethylene resin---50%;
(2) hydrophobic fumed nano silicon---50%;
(3) dispersion agent (TAF)----1%;
(4) 1010/168 oxidation inhibitor---0.2/0.2%.
This master batch is used for modifying plastics, and addition is 10% to get final product.
Embodiment 3
Modifying plastics nano silicon formula of master batch (weight percentage)
(1) grafted polyethylene resin---60%;
(2) hydrophobic fumed nano silicon---40%;
(3) dispersion agent (TAF)----1%;
(4) 1010/168 oxidation inhibitor---0.2/0.2%.
This master batch is used for modifying plastics, and addition is 12% to get final product.
Above-described embodiment only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the personage who is familiar with technique can understand content of the present invention and according to this enforcement, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (4)
1. a modifying plastics is with gas phase nano silicon-dioxide master batch and preparation method thereof, it is characterized in that: it is the synthetic silicon-dioxide of a kind of special process, it is synthetic under the pyrohydrolysis adopting vapor phase process, through special surface treatment, compound with grafted polyethylene (g-PE) again, form through water cycle or cold drawn bar pelletizing.
2. a kind of modifying plastics according to claim 1 is characterized in that described fumed silica synthesis technique is with gas phase nano silicon-dioxide master batch and preparation method thereof:
With the fumed silica of aforesaid method preparation, the particle diameter 7-40 nanometer of its primary particle, the large 50-380 ㎡/g of specific surface area, purity SiO2＞99.8%, general apparent density 50g/l.
3. a kind of modifying plastics according to claim 1 is with gas phase nano silicon-dioxide master batch and preparation method thereof, it is characterized in that described special surface treatment refers to above-mentioned fumed silica, be octamethylcyclotetrasiloxane with special treatment agent, under certain temperature condition, fully mix processing with the homogenizer more than 1000 rev/mins, so that its surperficial siloxanes and silanol and silane and silazane reaction, chemical modification occurs, become hydrophobic (lipophilic) property silicon-dioxide, can improve the wetting property between aerosil particle and the organic molecule, dispersed, interface bond strength, improve the over-all properties of matrix material, widen the Application Areas of product.
4. a kind of modifying plastics according to claim 1 is characterized in that the preparation method is with gas phase nano silicon-dioxide master batch and preparation method thereof:
The silicon-dioxide of above-mentioned processing and the polyethylene of maleic anhydride graft (g-PE) are mixed; through twin screw extruder; the adjusting engine speed is 180 ~ 350rpm; the feeding rotating speed is 250 ~ 800rpm; melt extrude temperature in 160 ~ 250 ℃ of scopes; under the conveying and shearing action of twin screw extruder; abundant fusion plastification; mediate mixing; water ring pelletizing or cold drawn bar pelletizing after head is extruded; packing namely gets modifying plastics with gas phase nano silicon-dioxide master batch after dry, so that silicon-dioxide is realized twice dispersing in modifying plastics is used, reaches better dispersion effect; simultaneously easy to use, environmental friendliness.
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| CN103881135A (en) * | 2014-03-15 | 2014-06-25 | 宿州学院 | Reinforced modified nano-silica masterbatch |
| US10836908B2 (en) | 2018-02-01 | 2020-11-17 | Dow Silicones Corporation | Composition, polymer composite article formed therewith, and method of preparing same |
| CN112708205A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Low-odor impact-resistant scratch-resistant polypropylene composition and preparation method thereof |
| CN112708204A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Toughened high-performance polypropylene composition and preparation method thereof |
| US11312861B2 (en) | 2019-08-07 | 2022-04-26 | Dow Silicones Corporation | Solid carrier component including a liquid polyorganosiloxane and methods for preparation and use of the solid carrier component |
| US11312862B2 (en) | 2019-08-07 | 2022-04-26 | Dow Silicones Corporation | Solid carrier component including a liquid polydiorganosiloxane and methods for preparation and use of the solid carrier component |
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| CN115029018A (en) * | 2022-06-13 | 2022-09-09 | 河南海博瑞硅材料科技有限公司 | High-stability hydrophobically modified nano silicon dioxide and preparation method thereof |
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| CN103881135A (en) * | 2014-03-15 | 2014-06-25 | 宿州学院 | Reinforced modified nano-silica masterbatch |
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| US10836908B2 (en) | 2018-02-01 | 2020-11-17 | Dow Silicones Corporation | Composition, polymer composite article formed therewith, and method of preparing same |
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| US11859086B2 (en) | 2019-08-07 | 2024-01-02 | Dow Silicones Corporation | Polydiorganosiloxane compositions and methods for use thereof in forming wood plastic composites |
| US11312861B2 (en) | 2019-08-07 | 2022-04-26 | Dow Silicones Corporation | Solid carrier component including a liquid polyorganosiloxane and methods for preparation and use of the solid carrier component |
| US11312862B2 (en) | 2019-08-07 | 2022-04-26 | Dow Silicones Corporation | Solid carrier component including a liquid polydiorganosiloxane and methods for preparation and use of the solid carrier component |
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