CN103881420B - The preparation method of a kind of starch/white carbon black compounded mix - Google Patents

The preparation method of a kind of starch/white carbon black compounded mix Download PDF

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CN103881420B
CN103881420B CN201410137384.1A CN201410137384A CN103881420B CN 103881420 B CN103881420 B CN 103881420B CN 201410137384 A CN201410137384 A CN 201410137384A CN 103881420 B CN103881420 B CN 103881420B
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starch
carbon black
white carbon
compounded mix
gelatinization
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CN103881420A (en
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王益庆
刘佳音
邓斯奇
沈家锋
张莉
张立群
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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Abstract

The present invention relates to the preparation method of a kind of starch/white carbon black compounded mix, the method is white carbon black to be mixed in the good starch paste of gelatinization in advance, be uniformly dispersed under certain mechanical shearing stirring action and temperature condition, oven dry granulation, pyroprocessing obtain starch/white carbon black compounded mix.The method modified technique is easy, environment friendly and pollution-free.In method of modifying involved in the present invention, the polyhydroxy structure of starch can form coating layer with the intermolecular generation physics chemical action of white carbon black, and the coated of these starch polymer chains improves the consistency of part white carbon black in sizing material.In mixing process, processing characteristics is obviously improved, dust reduction; Mechanical property also gets a promotion.

Description

The preparation method of a kind of starch/white carbon black compounded mix
Technical field
The present invention relates to the preparation method of a kind of starch/white carbon black compounded mix, especially the preparation of the special high-dispersity white carbon black of rubber materials.
Technical background
White carbon black and hydrated SiO 2, molecular formula is SiO 2nH 2o is a kind of white, nontoxic, unformed fines thing, have porousness, polymolecularity, light weight, chemical stability good, high temperature resistant, do not burn, the important inorganic silicon compound of the excellent properties such as electrical insulating property is good.Its relative density is 2.319 ~ 2.653, fusing point 1750 DEG C, is mainly used as the weighting agent of the products such as rubber, plastics, synthetic resins and paint.Wherein, the white carbon black of total amount 70% is accounted for for rubber industry.
White carbon black has special surface tissue (with surface hydroxyl and planar water), special particle form (particle is little, specific surface area is large) and unique physical and chemical performance.But the activated silica alcohol radical existed due to poly-silica and the outside surface of its inside and planar water thereof, make it be wetting ability, is difficult to moistening and dispersion in organic phase, and because its surface exists hydroxyl, surface energy is larger, aggregate always tends to cohesion, and thus the application performance of product is affected.For this reason, need to carry out surface modification to white carbon black, to improve its effect, improve value-added content of product, expand the Application Areas of product.
At present, the industrialization technology of white carbon black modification is mainly divided into wet-process modified and dry method modification.Wet-process modified is white carbon black heated and boiled together with properties-correcting agent and certain solution, is then separated dry process.Conventional properties-correcting agent is generally silane coupling agent, and the modifying function of coupling agent has also come by mixing front wet-process modified white carbon black by the direct interpolation in mixing process, and the two modified effect is suitable.
The in-situ modified correlation technique preparing white carbon black compounded mix of starch involved in the present invention there is no report at home and abroad at present.
Summary of the invention
Present invention utilizes the polyhydroxy structure on starch surface and white carbon black to act on altogether and prepare compounded mix.The silicone hydroxyl generation physical/chemical effect on starch and white carbon black surface thus improve its hydrophobic performance.The compounded mix obtained is dust to be reduced, and processing characteristics gets a promotion; Decrease the reunion of white carbon black, be easy to dispersion; Be enhanced with the consistency of rubber, filler gum mechanical property gets a promotion.
A preparation method for starch/white carbon black compounded mix, its key step is: be mixed into by white carbon black in the good starch paste of gelatinization in advance, and the mass ratio of solid white carbon black and starch is 20/1-5/1; Be uniformly dispersed under 60-90 DEG C of temperature condition, dry at 60-105 DEG C, granulation, processes 0.5-24h and obtains starch/white carbon black compounded mix at 180-250 DEG C.
As preferably: starch is W-Gum, yam starch, pea starch, green starch, glutinous rice starch, sweet potato starch, sweet potato starch, tapioca (flour), wheat starch.
As preferably: white carbon black is white carbon black powder or white carbon black slurries.
As preferably: the mass concentration of starch paste is 5%-20%.
Beneficial effect
1) preparation method's technique of starch involved in the present invention/white carbon black compounded mix is simple, the lower and energy-conserving and environment-protective of cost;
2) obtained compounded mix is dust to be reduced, and improves processing characteristics;
3) part reduces the reunion of white carbon black, is easy to dispersion;
4) compounded mix its fill glue mechanical property and compare pure white carbon black filled glue and get a promotion.
Embodiment
Embodiment 1:
100g W-Gum to be added in the water of 1900g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward the white carbon black powder being wherein mixed into 100g; Under 60 DEG C of conditions, make the two be uniformly dispersed; Dry at 105 DEG C, granulation; At 180 DEG C, pyroprocessing 24h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber after sulfuration.
Embodiment 2:
100g yam starch to be added in the water of 900g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward the white carbon black powder being wherein mixed into 150g; Under 70 DEG C of conditions, make the two be uniformly dispersed; Dry at 90 DEG C, granulation; At 190 DEG C, pyroprocessing 18h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber after sulfuration.
Embodiment 3:
150g pea starch to be added in the water of 850g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward the white carbon black powder being wherein mixed into 150g; Under 80 DEG C of conditions, make the two be uniformly dispersed; Dry at 75 DEG C, granulation; At 200 DEG C, pyroprocessing 12h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber after sulfuration.
Embodiment 4:
100g green starch to be added in the water of 400g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward the white carbon black powder being wherein mixed into 100g; Under 90 DEG C of conditions, make the two be uniformly dispersed; Dry at 60 DEG C, granulation; At 250 DEG C, pyroprocessing 2h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber after sulfuration.
Embodiment 5:
100g glutinous rice starch to be added in the water of 1900g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward the white carbon black powder being wherein mixed into 75g; Under 80 DEG C of conditions, make the two be uniformly dispersed; Dry at 60 DEG C, granulation; At 250 DEG C, pyroprocessing 2h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber after sulfuration.
Embodiment 6:
100g wheat starch to be added in the water of 900g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward the white carbon black powder being wherein mixed into 100g; Under 90 DEG C of conditions, make the two be uniformly dispersed; Dry at 75 DEG C, granulation; At 230 DEG C, pyroprocessing 9h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber after sulfuration.
Embodiment 7:
150g sweet potato starch to be added in the water of 850g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward the white carbon black powder being wherein mixed into 75g; Under 80 DEG C of conditions, make the two be uniformly dispersed; Dry at 90 DEG C, granulation; At 180 DEG C, pyroprocessing 21h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber after sulfuration.
Embodiment 8:
100g sweet potato starch to be added in the water of 400g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward the white carbon black powder being wherein mixed into 400g; Under 70 DEG C of conditions, make the two be uniformly dispersed; Dry at 75 DEG C, granulation; At 240 DEG C, pyroprocessing 0.5h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber after sulfuration.
Embodiment 9:
100g tapioca (flour) to be added in the water of 1900g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward being wherein mixed into the white carbon black slurries that 100g massfraction is 50%; Under 60 DEG C of conditions, make the two be uniformly dispersed, dry at 75 DEG C, granulation, at 190 DEG C, pyroprocessing 9h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber postcure.
Embodiment 10:
100g W-Gum to be added in the water of 900g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward being wherein mixed into the white carbon black slurries that 100g massfraction is 50%; Under 70 DEG C of conditions, make the two be uniformly dispersed, dry at 90 DEG C, granulation, at 200 DEG C, pyroprocessing 3h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber postcure.
Embodiment 11:
150g wheat starch to be added in the water of 850g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward being wherein mixed into the white carbon black slurries that 600g massfraction is 50%; Under 80 DEG C of conditions, make the two be uniformly dispersed, dry at 90 DEG C, granulation, at 230 DEG C, pyroprocessing 1h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber postcure.
Embodiment 12:
100g yam starch to be added in the water of 400g gelatinization 1h under the condition of 80 DEG C; Get the starch solution that 100g gelatinization is good, toward being wherein mixed into the white carbon black slurries that 200g massfraction is 50%; Under 80 DEG C of conditions, make the two be uniformly dispersed, dry at 105 DEG C, granulation, at 200 DEG C, pyroprocessing 3h obtains starch/white carbon black compounded mix; Compounded mix is surveyed its mechanical property by specified mix and compounding rubber postcure.
Comparative example:
Goldschmidt chemical corporation is produced VN3 type white carbon black and is filled glue.
In table 1, embodiment and comparative example, glue performance test results filled by white carbon black
In table 2, embodiment and comparative example, glue formula filled by white carbon black
Material Mass parts
SBR1502 100
ZnO 5
SA 2
Modified filler 67
Anti-4020NA 1
Si69 3
CZ 1.2
S 1.5
Note: the lifting of this modified filler performance is applicable to the various tread glue formula containing butylbenzene, suitable fourth, natural rubber, and embodiment only lists above-mentioned formula with for referencial use.

Claims (3)

1. a preparation method for starch/white carbon black compounded mix, is characterized in that: be mixed into by white carbon black in the good starch paste of gelatinization in advance, and the mass concentration of starch paste is 5%-20%;
The mass ratio of solid white carbon black and starch is 20/1-5/1; Be uniformly dispersed under 60-90 DEG C of temperature condition, dry at 60-105 DEG C, granulation, processes 0.5-24h and obtains starch/white carbon black compounded mix at 180-250 DEG C.
2. the preparation method of starch/white carbon black composite material according to claim 1, is characterized in that: starch is W-Gum, yam starch, pea starch, green starch, glutinous rice starch, sweet potato starch, sweet potato starch, tapioca (flour), wheat starch.
3. the preparation method of starch/white carbon black composite material according to claim 1, is characterized in that: white carbon black is white carbon black powder or white carbon black slurries.
CN201410137384.1A 2014-04-07 2014-04-07 The preparation method of a kind of starch/white carbon black compounded mix Active CN103881420B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103387696A (en) * 2013-07-29 2013-11-13 海南大学 In-situ polymerization method of nano starch/SiO2 composite particles

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103387696A (en) * 2013-07-29 2013-11-13 海南大学 In-situ polymerization method of nano starch/SiO2 composite particles

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