CN107857900B - The preparation method of rubber filling, rubber filling and application thereof - Google Patents

The preparation method of rubber filling, rubber filling and application thereof Download PDF

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CN107857900B
CN107857900B CN201710154413.9A CN201710154413A CN107857900B CN 107857900 B CN107857900 B CN 107857900B CN 201710154413 A CN201710154413 A CN 201710154413A CN 107857900 B CN107857900 B CN 107857900B
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filler
coal gasification
rubber
fine slag
separation
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CN107857900A (en
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魏存弟
艾卫东
薛兵
蒋引珊
徐少南
夏茂盛
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Ordos Huiheng Technology Co., Ltd
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Jilin University
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K11/00Use of ingredients of unknown constitution, e.g. undefined reaction products
    • C08K11/005Waste materials, e.g. treated or untreated sewage sludge
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/08Ingredients of unknown constitution and ingredients covered by the main groups C08K3/00 - C08K9/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/09Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/16Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/06Properties of polyethylene
    • C08L2207/066LDPE (radical process)

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Abstract

The method of rubber filling, rubber obtained, filler and application thereof are prepared using coal gasification fine slag the invention discloses a kind of, which comprises take appropriate coal gasification fine slag, water is added to prepare the coal gasification fine slag slurry for being contained in 10-30wt% admittedly;The slurry of configuration is sufficiently stirred, it later by gravity cyclonic separation, collects heavy separation product and obtains the compound slurry of Silicon-rich, and the Silicon-rich composite mortar is separated by solid-liquid separation and is dried, it wherein, further include screening process before the separation of solid and liquid or after being dried;The invention also discloses rubber products or plastic products that offer is prepared using above-mentioned filler.Filler of the invention can be directly used in the preparation of product of rubber and plastic under the conditions of without organically-modified, play rheological agent effect, improve its processing performance;Play the role of reinforcing agent in products obtained therefrom, improve the intensity of product, hardness, ageing resistance and improve its high-temperature stability, realizes the high value added product exploitation of coal gasification fine slag.

Description

The preparation method of rubber filling, rubber filling and application thereof
Technical field
The invention belongs to the technical scopes that solid waste resource recovery utilizes, in particular to a kind of to utilize coal gasification fine slag system The method of standby rubber filling, rubber filling obtained and application thereof, and the product of rubber and plastic being prepared using above-mentioned filler.
Background technique
Coal Gasification Technology is one of the core content of clean coal technology, and coal is carried out incomplete oxidation to obtain for downstream Utilize can coal-fired gasification gas (such as raw gas), in recent years quickly become coal resources and using energy source important directions.Closely Over 20 years, China mostly has built a collection of coal chemical industry enterprises in Yulin, Ordos, inner Mongolia, Shanxi Changzhi etc., It goes into operation successively, yield increases year by year, and the clean comprehensive utilization of coal resources takes on a certain scale in China.
In Coal Gasification Technology system, by while carbonaceous part is largely converted into gas in coal, association in raw coal Inorganic mineral components, the catalyst of addition and gasification are not thorough remaining carbonaceous and can be arranged in the form of residue (coal gas slugging) Out.Because the difference of mode is discharged, coal gas slugging is divided into thick slag and fine slag again, wherein the thick slag refers to via coal gasifier The residue of furnace bottom discharge, and fine slag refers to and is carried secretly by coal gasification gas and in the purification process after coal gasification gas leaves coal gasifier Separate the residue of discharge.The yield of coal gasification residue increases quickly with the development of Chemical Industry, land occupation when stacking, Environment is polluted, new solid waste urgently to be resolved is had become.
In recent years, started the concern for causing some scholars around the utilization of coal chemical industry slag.201510148929.3 disclosure of CN A kind of light ceramic and its methods and applications processed using the gentle slugging preparation of flyash, describes and utilizes flyash and gasification Slag prepares light ceramic and its preparation method;CN 201510420421.4 disclose it is a kind of for produce the composition of ceramic for filtration with And ceramic for filtration and its preparation method and application, describe the method for preparing ceramic for filtration using gasification slag for main component;CN 201310207509.9 disclose the method that activation coal gasification lime-ash realizes the separation of ferro-aluminum calcium, describe coal gas slugging is dry Afterwards, chilling obtains activated material after being calcined at 700 to 1100 DEG C 75 minutes, then by activated material and hydrochloric acid solution or sulfuric acid solution Reaction realizes aluminium, iron, Calcium compounds separation, and can use the calorific value of carbon residue in coal gasification lime-ash;CN 201210511610.9 disclose a kind of processing method of coal chemical industry gasification slag, describe the gentle slugging of coal slime after evenly mixing Clay wash is added, using high-pressure pump pipe conveying technology, mixture is transported in the fluidized-bed combustion boiler furnace outside hundreds of meters, is led to Cross the utilization of burning again that fluidized-bed combustion boiler combustion technology realizes gasification slag;Shenhua Ningxia Coal Industry Group Co., Ltd. Yang Shuai and Shi Lijun publishes an article in August, 2013 " coal chemical industry " in, describes Shenhua Ningxia Coal Industry Group Co., Ltd .'s coal chemical industry Various oxide component contents and loss on ignition in 3 kinds of coal gasification fine slags of output, in conjunction with total utilization of PCA national standard and Professional standard has carried out feasibility analysis for cement, concrete, building materials and road foundation blend composition etc. to coal gasification fine slag, It proposes coal gasification fine slag and mixes the suggestion for burning that utilization and sorting utilize;Liu Ziliang etc. is total using having carried out both at home and abroad to gasification slag Knot is included in sewage treatment, builds the road, is non-burning brick, applying in cement and concrete etc..Data from recent years shows, Ren Menyi It is recognized the harm of coal gas slugging, starts its composed structure of system research from different perspectives and characteristic, and start to pay attention at its It sets and Utilizing question.
It is comprehensive about the research report of coal gasification slag it is found that existing utilize about coal gasification body refuse, mainly for The wherein other components such as sa inorganic component other than the higher charcoal of content, only a few studies are reported coal gas slugging weight New mixing is coal-fired to be used as fuel treatment, is seldom related to the development and utilization of wherein rich charcoal component.In fact, gasification slag in sa The charcoal coexisted can also have an impact the performance of sial component.
Since the 1990s, people just recognize that inorganic particle improves rubber and plastic system for that can become among rubber and plastic Moral character can and reduce the effective way of cost, in addition to the carbon black and white carbon black powder dedicated for filler, such as aluminium oxide, carbonic acid The oxides such as calcium, talcum, kaolinite, montmorillonite powder and silicate powder, which are also studied, to be utilized.Inorganic filler is dosed in rubber and plastic Raw rubber or resin usage amount can be reduced, anti-flammability is improved, increases hardness and mechanical strength and reduce cost, obtained universal Using.It is good to obtain filler compatibility but since the surface polarity of inorganic powder particle influences its dispersibility in the polymer Effect, generally require to carry out surface organics coating modification, however, this can also correspondingly increase cost simultaneously.In recent years, with people To solid waste comprehensive utilization attention, it is also more and more to its processing modified research on utilization as rubber filling, close In mineral surface modification and its in rubber and plastic using having considerable report, as the Zhang Yun of University Of Chongqing cherishes doctor (2004) It conducts a research specifically for fly ash micro-sphere surface organic modification as rubber filling;Liu Shan (2012) changes fly ash micro-sphere Property PVC composite material has carried out experimental study etc..About carbon to inorganic powder surface polarity improvement result, in patent 200910218038.5, in 201110355054.6 and 201210288939.3, respectively in diatomite, oil shale waste and flyash Carbon has been paid close attention in acid dissolution slag system and there is effect to powder just face performance, but related method does not account for its particle shape The influence of convection current change craftsmanship.
So far, it yet there are no for coal gasification fine slag medium high carbon content microballon without modified directly as rubber or modeling The relevant report of stream change supporting material.
Summary of the invention
The one side of the purpose of the present invention is to provide a kind of method using the preparation gum filler of coal gasification fine slag, is made Gum filler and application thereof, filler prepared in accordance with the present invention can be without organically-modified and direct compared with conventional filler Preparation for rubber product or plastic products, it is possible to reduce or without using traditional compatilizer.
The purpose of the present invention further aspect is that providing the rubber product being prepared using above-mentioned filler or plastics system Product.Filler of the invention can play rheological agent effect well, improve its processing performance, in addition it can in products obtained therefrom Play the role of reinforcing agent, improve the intensity of product, hardness, ageing resistance and improve its high-temperature stability, realizes coal gasification fine slag High value added product development and utilization.
The method provided by the invention for preparing rubber filling using coal gasification fine slag, adopts the following technical scheme that
A method of rubber filling is prepared using coal gasification fine slag, which comprises
A, appropriate coal gasification fine slag is taken, water is added to prepare the coal gasification fine slag slurry for being contained in 10-30wt% admittedly;
B, the slurry of step a configuration is sufficiently stirred, later by gravity cyclonic separation, collects heavy separation product The compound slurry of Silicon-rich is obtained, and the Silicon-rich composite mortar is separated by solid-liquid separation and is dried, wherein in the solid-liquid It further include screening process before separation or after being dried, to separate big in the Silicon-rich composite mortar or desciccate Grain makes the granularity of gained powder be not more than 200 mesh (i.e. granularity is less than or equal to partial size corresponding to 200 mesh Taylor standard sieves), with As rubber filling.
In the present invention, the coal gasification fine slag is to be carried secretly by coal gasification gas and after coal gasification gas leaves coal gasifier The residue of separation discharge in purification process (such as through cyclone dust removal, bag-type dust and/or washing), coal gasification course is this field It is known, it will be appreciated by those skilled in the art that the inorganic mineral composition of pit ash is primarily formed as contained in feed coal, with And be not gasified totally and remaining charcoal in gasification, inevitably carry solid phase group in coal gasification gas caused by coal gasification secretly Point, wherein the lesser solid phase components of granularity leave gasification furnace and form coal gasification fine slag, and all components are amorphous state, and partial size is little In 120 μm.
In step a of the invention, when being mixed and made into slurry using coal gasification fine slag and water, those skilled in the art's reason Solution, the gasification fine slag can be dry slag and be also possible to wet slag, make the solid content of slurry in 10wt%~30wt%, preferably 15wt%~25wt%, such as 20wt%.In a preferred embodiment, after the coal gasification fine slag slurry at least 1h of configuration Subsequent stir process, such as 1.5h, 2h or 5h are carried out again, are come into full contact with, are soaked with water so that coal gasification is refined, thus favorably In subsequent cyclonic separation.
In step b in the present invention, slurry is stirred, then cyclonic separation obtains the compound slurry of Silicon-rich;Wherein, The stirring is processing means commonly used in the art, such as can be stirred using mixing plant, it is preferred to use reinforcement Blender is stirred.In a preferred embodiment, in the preparation process of Silicon-rich composite mortar, stirring condition is that stirring turns Speed is not less than 1500r/min, and mixing time is no less than 30min;Preferably, speed of agitator is 1800~3000r/min, when stirring Between be 60min~180min;In order to subsequent cyclonic separation.The study found that by above-mentioned strong stirring, especially for leaching Bubble treated pulp separation better effect.Cyclonic separation is processing means commonly used in the art, such as can be using eddy flow point Cyclonic separation is carried out from device, in cyclonic separation, due to gravity, the lesser charcoal component of density is mainly from eddy flow point in fine slag It is overflowed from the top of device, and the biggish sa component of density (heavy separation product) is then mainly discharged from bottom, divides to realize From.
In step b of the invention, resulting Silicon-rich composite mortar is subsequent will also to carry out being separated by solid-liquid separation and to separating obtained Solid phase is dried, and above-mentioned treatment process is known in the art, such as slurry is carried out plate compression or centrifuge separation, Then obtained solid product is obtained into desciccate in 60-110 DEG C of dry 4-8h;Wherein, before the separation of solid and liquid or dry Further include screening process after dry processing, such as the Silicon-rich composite mortar is sieved using vibrating screen before separation of solid and liquid Divide processing, to separate the bulky grain in the Silicon-rich composite mortar, or after drying treatment using vibrating screen directly to dry Dry product carries out screening process, to separate the bulky grain in desciccate.In the present invention, by above-mentioned screening process, make most The granularity of gained powder is not more than 200 mesh, preferably no greater than 300 mesh, such as 250 or 350 mesh eventually, for use as rubber product or modeling Filler in material products.
In the present invention, although handling by eddy flow, charcoal component in part can be still contained in the Silicon-rich composite mortar.By In coal gasification reaction belong to coal incomplete oxidation reaction, remain charcoal in gasification with reducing atmosphere (coal gasification gas, Also referred to as synthesis gas or raw gas) continuous contact at high operating temperatures, so that form, activity of charcoal etc. be not in coal gasification fine slag The residual carbon being same as in conventional coal-fired ashes, research find that after processing part charcoal is coated on gasification slag bead surface, favorably In reducing the glass microballoon surface polarity in powder, improve the compatibility with rubber and plastic macromolecule material, give full play to rheology and Supplement effect.
In one embodiment of the present invention, in filler powder carbon content be not less than 5wt%, such as 8-20wt%, 10wt%, 15wt% or 18wt%.For carbon content in the solid phase of powder or the compound slurry of Silicon-rich, those skilled in the art's reason Solution can be controlled by modes such as the charging angle of adjusting cyclone or feed rates, to increase or decrease carbon therein Component.
Filler provided by the invention is the filler being prepared by the above method.
The present invention also provides above-mentioned fillers to prepare the application in rubber product or plastic products.
The present invention also provides a kind of rubber products, are prepared by the raw material for including raw rubber, filler and additive, described Filler is 0.65~1:1, such as 0.8:1 with the dosage mass ratio of the raw rubber, and the filler include the first filler and Second filler, first filler are carbon black, and second filler is rubber filling of the invention;Preferably, it described second fills out The mass ratio of material and the first filler is not more than 1:1, preferably 1:2~1:9, such as 1:3 or 1:4;Wherein the additive can be with It is rubber additive commonly used in the art, such as vulcanizing agent and antioxidant etc., is known in the art;The rubber product preparation Mixing and moulding process be it is known in the art, which is not described herein again.
The present invention also provides a kind of plastic products, are prepared by the raw material for including resin, filler and additive, described Filler is filler as claimed in claim 7;Preferably, in terms of the total amount of raw material, the dosage of the filler is 5~50wt%, than Such as 10wt%, 20wt%, 30wt% or 40wt%;Wherein the additive can be plastic products addition commonly used in the art Agent, such as antioxidant etc. are known in the art;The mixing of the plastic products preparation and moulding process are ripe for this field Know, which is not described herein again.
Compared with prior art, the invention has the following advantages that
1, in the present invention, coal gasification fine slag used be coal after high-temperature gasification by the nothing of wherein main siliceous, aluminium etc. Machine minerals conversion at amorphous silicon aluminum substance (while also containing calcium, iron etc.) and residual charcoal mixture, with conventional fire coal Ashes are different, since coal gasification reaction belongs to the incomplete oxidation reaction of coal, remain charcoal in gasification with reproducibility gas Continuous contact, the process are similar to the activation of coal to atmosphere (coal gasification gas, also referred to as synthesis gas or raw gas) at high operating temperatures Processing, so that form, activity of charcoal etc. are different from the remaining char in conventional coal-fired ashes in coal gasification fine slag.And this hair Microballon significant difference in bright coal gasification fine slag in microballon and flyash is that its component all exists with amorphous state state, and portion Unformed charcoal is divided to be distributed in glass microballoon surface, so that the polar character of sial glass microballoon is alleviated, with rubber and resin Compatibility it is good, it is not necessary that rubber and plastic supporting material can be become in organically-modified situation, prepare plastic products and rubber It can lack in product with even without compatilizer or modifying agent;
2, the present invention is acted synergistically in fine slag by many kinds of measures, realizes the separation of bulky grain charcoal and sial metallic substance, Good separation;And coal gasification solid impurity particle is fine, and the fine slag after separation helps to reduce polarity, improves phase without being crushed Capacitive;
3, using method of the invention, the carbon containing glass microballoon in coal gasification fine slag can be made without organically-modified item The preparation of product of rubber and plastic is directly used under part, the spherical state of sa microballon in fine slag is distributed in linear high molecular material Moving resistance is small, can play rheological agent effect, improve its processing performance, reduces abrasion of the material to equipment container material;It is spherical The good dispersion of particle, plays the role of reinforcing agent in products obtained therefrom, can improve the intensity, hardness, ageing resistance of product simultaneously Its high-temperature stability is improved, realizes the high value added product exploitation of coal gasification fine slag.
Specific embodiment
Below with reference to embodiment, the present invention is described in detail, but the present invention is not limited to this.
In following embodiment/comparative example, coal gasification fine slag used is from the industry of Ordos, inner Mongolia Jungar Banner main road Garden, property/combination are as follows: carbon content is about 38wt%, and silica is about 25wt%, and all components are amorphous state, grain Diameter is less than 120 μm.
Embodiment 1
100g coal gasification fine slag (wherein aqueous 55wt%) is weighed, being diluted with water to solid content is 20wt%, is adopted under room temperature It is stirred with high velocity dispersators (Foshan Yi Fu Machinery Co., Ltd.), speed of agitator 1800r/min, mixing time is 30min;Slurry is imported in cyclone separator and is separated, obtained lower part slurry is Silicon-rich composite mortar, is set using vibrating screen It is standby that screening process is carried out to Silicon-rich composite mortar, then slurry is separated by solid-liquid separation, filter cake is moved into dry in 110 DEG C of baking ovens 6h obtains filler powder, and carbon content is 14wt% in the powder, and grain diameter is not more than 300 mesh;
Natural rubber raw rubber 15g is weighed, takes filler powder 2.5g, semi-reinforcing hydrocarbon black 7.5g, additive: zinc oxide 0.61g, Stearic acid 0.2g, sulphur 0.2g and vulcanization accelerator TMTD 0.2g;By above-mentioned material under the conditions of 80 DEG C of kneading machine, revolving speed It for 32r/min, is kneaded after 25min, in 130 DEG C of vulcanization 25min, obtained sample placement tests its tensile strength afterwards for 24 hours and is 27.0MPa(GB/T528-2009)。
Comparative example 1
The difference from embodiment 1 is that the filler powder in embodiment 1 is replaced with etc. to the semi-reinforcing hydrocarbon black of quality, His process is identical with condition, and obtained sample tensile strength is 23.6MPa.
Embodiment 2
100g coal gasification fine slag (wherein aqueous 55wt%) is weighed, being diluted with water to solid content is 20wt%, is adopted under room temperature It is stirred with high velocity dispersators (Foshan Yi Fu Machinery Co., Ltd.), speed of agitator 1600r/min, mixing time is 40min;Slurry is imported in cyclone separator and is separated, obtained lower part slurry is Silicon-rich composite mortar, is set using vibrating screen It is standby that screening process is carried out to Silicon-rich composite mortar, then slurry is separated by solid-liquid separation, filter cake is moved into dry in 110 DEG C of baking ovens 6h obtains filler powder, and carbon content is 13wt% in the powder, and grain diameter is not more than 300 mesh;
Ethylene propylene diene rubber raw material 13.3g is weighed, takes filler powder 3.76g, semi-reinforcing hydrocarbon black 8.79g, additive: oxidation Zinc 0.67g, stearic acid 0.2g, atoleine 6g, sulphur 0.2g, DCP 0.8g and vulcanization accelerator TMTD 0.2g;It will be above-mentioned Material is under the conditions of 85 DEG C of kneading machine, revolving speed 30r/min, is kneaded after 25min, and sample suppresses 5 times in open mill, then Hot-forming under 10MPa at 130 DEG C, it is 9.12MPa that its tensile strength is tested in obtained sample placement afterwards for 24 hours;
Comparative example 2
The difference from example 2 is that the filler powder in embodiment 2 is replaced with etc. to the semi-reinforcing hydrocarbon black of quality, His process is identical with condition, and obtained sample tensile strength is 8.54MPa.
Embodiment 3
100g coal gasification fine slag (wherein aqueous 55wt%) is weighed, being diluted with water to solid content is 20wt%, is adopted under room temperature It is stirred with high velocity dispersators (Foshan Yi Fu Machinery Co., Ltd.), speed of agitator 1500r/min, mixing time is 40min;Slurry is imported in cyclone separator and is separated, obtained lower part slurry is Silicon-rich composite mortar, is set using vibrating screen It is standby that screening process is carried out to Silicon-rich composite mortar, then slurry is separated by solid-liquid separation, filter cake is moved into dry in 110 DEG C of baking ovens 6h obtains filler powder, and carbon content is 16wt% in the powder, and grain diameter is not more than 300 mesh;
30g PE particulate material is weighed, filler powder is added, so that its content is reached the 10wt% of total amount, in kneading machine 170 DEG C of mixing 30min, revolving speed 50r/min, obtained sample is placed at room temperature to be tested its tensile strength afterwards for 24 hours and is 19.02MPa。
Comparative example 3
Identical as the condition of embodiment 3, difference is, doses commercially available 6000 mesh calcium carbonate powder, makes the total inventory of its Zhan 10wt%, be added antioxidant (propionic acid n-octadecyl alcohol ester) 0.3g, compatilizer (maleic anhydride grafting low density polyethylene (LDPE)) 1.5g, other processes are identical with condition, and obtained sample tensile strength is 17.35MPa.
Embodiment 4
100g coal gasification fine slag (wherein aqueous 55wt%) is weighed, being diluted with water to solid content is 20wt%, is adopted under room temperature It is stirred with high velocity dispersators (Foshan Yi Fu Machinery Co., Ltd.), speed of agitator 1500r/min, mixing time is 40min;Slurry is imported in cyclone separator and is separated, obtained lower part slurry is Silicon-rich composite mortar, is set using vibrating screen It is standby that screening process is carried out to Silicon-rich composite mortar, then slurry is separated by solid-liquid separation, filter cake is moved into dry in 110 DEG C of baking ovens 6h obtains filler powder, and carbon content is 16wt% in the powder, and grain diameter is not more than 300 mesh;
30g LDPE particulate material is weighed, filler powder is added, so that its content is reached the 40wt% of total amount, in kneading machine 170 DEG C of mixing 30min, revolving speed 50r/min, obtained sample is placed at room temperature to be tested its tensile strength afterwards for 24 hours and is 13.19MPa。
Comparative example 4
Difference with embodiment 4 is, doses commercially available 6000 mesh calcite in powder filler 40wt%, other processes and condition phase Together, the sample tensile strength obtained is 9.89MPa.
Embodiment 5
100g coal gasification fine slag (wherein aqueous 55wt%) is weighed, being diluted with water to solid content is 20wt%, is adopted under room temperature It is stirred with high velocity dispersators (Foshan Yi Fu Machinery Co., Ltd.), speed of agitator 1500r/min, mixing time is 40min;Slurry is imported in cyclone separator and is separated, obtained lower part slurry is Silicon-rich composite mortar, is set using vibrating screen It is standby that screening process is carried out to Silicon-rich composite mortar, then slurry is separated by solid-liquid separation, filter cake is moved into dry in 110 DEG C of baking ovens 6h obtains filler powder, and carbon content is 16wt% in the powder, and grain diameter is not more than 300 mesh;
ABS resin 30g, zinc stearate 1.5g, stearic acid 0.18g, EBS1.2g are uniformly mixed, and kneading machine heating is added, melts After melting, filler 3.5g is added;In 240 DEG C of mixings 15min, revolving speed 30r/min;By mixed material, through hot press molding after, Test tensile strength is 31.727MPa.
Comparative example 5
30g ABS particulate material is weighed, the commercially available calcium carbonate powder 3.5g of 6000 mesh is dosed, its amount of filling is made to reach total amount 10wt%, other additives are identical with condition, its tensile strength of obtained sample test is 26.842MPa.
Embodiment 6
100g coal gasification fine slag (wherein aqueous 55wt%) is weighed, being diluted with water to solid content is 20wt%, is adopted under room temperature It is stirred with high velocity dispersators (Foshan Yi Fu Machinery Co., Ltd.), speed of agitator 1500r/min, mixing time is 40min;Slurry is imported in cyclone separator and is separated, obtained lower part slurry is Silicon-rich composite mortar, is set using vibrating screen It is standby that screening process is carried out to Silicon-rich composite mortar, then slurry is separated by solid-liquid separation, filter cake is moved into dry in 110 DEG C of baking ovens 6h obtains filler powder, and carbon content is 16wt% in the powder, and grain diameter is not more than 300 mesh;
ABS resin 30g, zinc stearate 1.5g, stearic acid 0.18g, EBS1.2g are uniformly mixed, and kneading machine heating is added, melts After melting, filler 15g is added;In 240 DEG C of mixings 15min, revolving speed 30r/min;By mixed material, through hot press molding after, Test tensile strength is 22.2MPa.
Comparative example 6
30g ABS particulate material is weighed, the commercially available calcium carbonate powder 15g of 6000 mesh is dosed, its amount of filling is made to reach total amount 31wt%, other additives are identical with condition, its tensile strength of obtained sample test is 20.447MPa.

Claims (14)

1. a kind of method for preparing rubber filling using coal gasification fine slag, which comprises
A, appropriate coal gasification fine slag is taken, water is added to prepare the coal gasification fine slag slurry for being contained in 10-30wt% admittedly;
B, the slurry of step a configuration is sufficiently stirred, later by gravity cyclonic separation, collects heavy separation product and obtain The compound slurry of Silicon-rich, and the Silicon-rich composite mortar is separated by solid-liquid separation and is dried, wherein in the separation of solid and liquid It further include before or after being dried screening process, to separate the bulky grain in the Silicon-rich composite mortar or desciccate, Make the granularity of gained powder no more than 200 mesh for use as rubber, plastic filler;
Wherein, in step a, the coal gasification fine slag is to be carried secretly by coal gasification gas and net after coal gasification gas leaves coal gasifier The residue of separation discharge during changing;
In step b, stirring condition is that speed of agitator is not less than 1500r/min, and mixing time is no less than 30min.
2. the method according to claim 1, wherein carbon content is 8-20wt% in the powder in step b.
3. being stirred the method according to claim 1, wherein speed of agitator is 1800~3000r/min in step b Mixing the time is 40min~180min.
4. according to the method described in claim 3, it is characterized in that, after the coal gasification fine slag slurry at least 1h of step a configuration The stir process of step b is carried out again.
5. method according to any of claims 1-4, which is characterized in that in step b, before the separation of solid and liquid Carry out screening process.
6. according to the method described in claim 5, it is characterized in that, the granularity of gained powder is not more than 300 mesh in step b.
7. method according to any of claims 1-4, which is characterized in that the component of the coal gasification fine slag is non- Crystalline state, partial size are not more than 120 μm.
8. a kind of filler that the method is prepared according to claim 1~any one of 7.
9. filler as claimed in claim 8 is preparing the application in rubber product or plastic products.
10. a kind of rubber product, be prepared by the raw material for including raw rubber, filler and additive, the filler with the life The dosage mass ratio of glue is 0.65~1:1, and the filler includes the first filler and the second filler, and first filler is charcoal Black, second filler is filler according to any one of claims 8.
11. rubber product according to claim 10, which is characterized in that the mass ratio of second filler and the first filler No more than 1:1.
12. rubber product according to claim 11, which is characterized in that the mass ratio of second filler and the first filler For 1:2~1:9.
13. a kind of plastic products are prepared by the raw material for including resin, filler and additive, the filler is claim 8 The filler.
14. plastic products according to claim 13, which is characterized in that in terms of the total amount of raw material, the dosage of the filler For 5~50wt%.
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CN112916200B (en) * 2019-12-05 2022-06-17 山西奇色环保科技股份有限公司 Method for preparing plastic filler by taking gasified slag as raw material
CN113480779A (en) * 2021-05-21 2021-10-08 内蒙古万邦清源环保科技有限公司 Method for preparing composite carbon superfine powder material for rubber by using gasified slag
CN113308025A (en) * 2021-05-25 2021-08-27 内蒙古万邦清源环保科技有限公司 Method for directly preparing high-activity micro-nano superfine powder material for highway asphalt by utilizing gasified slag
CN113831594B (en) * 2021-10-29 2022-10-14 吉林大学 Composite filler taking coal gasification fine slag as raw material and preparation method and application thereof
CN114634672B (en) * 2022-03-22 2023-12-15 国家能源集团宁夏煤业有限责任公司 Polypropylene composition, polypropylene composite powder, preparation method and application thereof, and polypropylene product

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Inventor after: Wei Cundi

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