CN103554519B - A kind of preparation method of waste fluorine rubber powder of polymolecularity - Google Patents

A kind of preparation method of waste fluorine rubber powder of polymolecularity Download PDF

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Publication number
CN103554519B
CN103554519B CN201310553672.0A CN201310553672A CN103554519B CN 103554519 B CN103554519 B CN 103554519B CN 201310553672 A CN201310553672 A CN 201310553672A CN 103554519 B CN103554519 B CN 103554519B
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rubber powder
fluorine rubber
waste fluorine
waste
powder
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CN103554519A (en
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王兆波
王灿灿
李帅
王新
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Qingdao University of Science and Technology
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Qingdao University of Science and Technology
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Abstract

The present invention relates to a kind of preparation method of waste fluorine rubber powder of polymolecularity, comprise following order step: the waste fluorine rubber powder sieve pulverized under normal temperature, grinding obtains is separated by (1), obtain the rubber powder of different-grain diameter; (2) waste fluorine rubber powder is loaded in mixing equipment, add nano inorganic powder afterwards, realize the parcel process to vulcanized rubber powder by mixing; (3) take out in surface treated rubber powder slave unit, pack stores.The present invention carries out parcel process by adopting nano inoganic particle to the surface of waste fluorine rubber powder, efficiently solves the caking phenomenon that rubber powder particle occurs in put procedure, obtains a kind of waste fluorine rubber powder that can place for a long time with polymolecularity.The physically encapsulation degree on waste fluorine rubber powder surface easily controls, and surface treated rubber powder disperses easily in rubber mixing process, and can increase substantially loading level.The method is simple, and processing ease, has feasibility of batch preparation.

Description

A kind of preparation method of waste fluorine rubber powder of polymolecularity
Technical field
The present invention relates to a kind of preparation method of waste fluorine rubber powder of polymolecularity, be specifically related to a kind of preparation method suppressing the waste fluorine rubber powder of luming, specifically, relate to a kind of by the physically encapsulation process to waste fluorine rubber powder surface, solve the agglomeration problems of rubber powder, thus obtain the preparation method of the waste fluorine rubber powder of polymolecularity.
Background technology
Along with the development of science and technology, the consumption of whole world rubber is in rising tendency year by year, because waste rubber belongs to heat cured macromolecular material, be difficult under field conditions (factors) degrade, the accumulation of a large amount of waste old brings hidden trouble to global environment and public health security.The way of recycling of early stage waste old is mainly burning, thermo-cracking and landfill etc., and the recycling mode of the waste old of developing green environmental protection has been imperative.By waste old is made rubber powder, then using with other material blending is the optimal path that utilizes of rubber industry wastewater and the attractive method of most.
Waste old rubber powder take waste or used vulcanized rubber as raw material, pulverized or grind and make varigrained powdery substance by mechanical workout, and common production method is normal temperature crushing up, pulverize at low temperature method and solution comminuting method.In the production of current waste old rubber powder, normal temperature crushing up is occupied an leading position, and the output of waste-tyre rubber-powder occupy the first.Compared with waste-tyre rubber-powder, the rubber powder Synthesis and applications of waste and old specialty elastomer more causes the concern of people, viton is vinylidene fluoride (VDF), R 1216 (HFP), the copolymer of tetrafluoroethylene (TFE) or terpolymer, viton is widely used in preparing high performance sealing material with heat-resisting, oil resistant, the chemical mediator-resitant property of its excellence.Comparatively conventional rubber, viton price is high, and in the process of compression molding, discarded scrap stock are more, to the preparations and applicatio of the rubber powder of waste fluorine, have important commercial value.Based on the angle of economy, ambient ground, grinding is the most popular method of preparation waste fluorine rubber powder, the method can prepare the rubber powder of below 100 orders, but the waste fluorine rubber powder surface irregularity prepared by normal temperature grinding, engagement is produced after particle contact, and cause rubber powder at memory period, under self gravitation effect, there is the caking of waste fluorine rubber powder, and the broken difficulty of rubber powder after caking, this directly causes in the application process of follow-up rubber powder, caking rubber powder difficulties in dispersion, loading level is difficult to improve, have impact on applying of waste fluorine rubber powder.In CN200920244955.6 patent, for the caking phenomenon that rubber powder occurs after depositing after a while, propose a kind of shredding unit of lump rubber powder, but do not solve the problem depositing rubber powder caking in process.
Based on current research situation, the present invention adopts the pack of nanometer physical package, by the physically encapsulation on the coarse waste fluorine rubber powder surface of effects on surface, effectively suppresses the caking of rubber powder, obtain there is polymolecularity can the waste fluorine rubber powder of prolonged storage.
Goal of the invention and summary of the invention
The present invention is directed to the agglomeration problems of waste fluorine rubber powder in storage process of ambient ground, grinding preparation, propose a kind of preparation method of waste fluorine rubber powder of polymolecularity, the method is simple, the physically encapsulation degree on waste fluorine rubber powder surface easily controls, and imparts good batch production feasibility.
The invention provides a kind of preparation method of waste fluorine rubber powder of polymolecularity, comprise following order step:
(1) with sieve, the waste fluorine rubber powder that ambient ground, grinding obtain is separated, obtains the rubber powder of different-grain diameter;
(2) waste fluorine rubber powder is loaded in mixing equipment, add nano inorganic powder afterwards, under certain mixing condition, realize the physically encapsulation process to rubber powder uneven surface;
(3) take out in the waste fluorine rubber powder slave unit of surface parcel process, load in bag and preserve.
Wherein, described waste fluorine rubber powder be pulverize under normal temperature condition, the cross-linked rubber of the waste fluorine of grinding and the rubber powder that obtains; Mixing equipment is air driven mixer, drum mixer, double-cone mixer, kneader or high-speed mixer.
Described nano inorganic powder is any one or its arbitrary combination in precipitated silica, nano titanium oxide, nano zine oxide, nano-calcium carbonate.
The consumption of nano inorganic powder is 3 ~ 8% of waste fluorine rubber powder quality; Waste fluorine rubber powder and nano inorganic powder be blended in normal temperature condition under carry out; The mixing time adopting high-speed mixer is 5 ~ 10 minutes, and the mixing time adopting air driven mixer, drum mixer, double-cone mixer or kneader is 10 ~ 20 minutes.
In technique scheme, by the separation of pulverizing, grinding the waste fluorine rubber powder obtained, obtain the rubber powder of different-grain diameter, ensure that the uniform particle sizes of rubber powder; For the waste fluorine rubber powder of mechanical disintegration under normal temperature condition, grinding preparation, in process of lapping, the micelle severe friction that die head is very strong with being in the elasticity of elastomeric state, makes its particle diameter constantly reduce, but obtain the surface irregularity, uneven of rubber powder; When waste fluorine rubber powder loads in packing bag, in storage process, placement is piled up in packing bag, under the effect of rubber powder self gravitation, facilitate the physics engagement between shaggy waste fluorine rubber powder particle, and showing as bonding and the caking of rubber powder, even whole bag rubber powder lumps into as a whole; The particle diameter of rubber powder is less, lumps also more serious.For the caking of this waste fluorine rubber powder, usually adopt artificial hand to break and hand rubbing, little caking can only be broken into, the rubber powder with good distribution behavior of powdery can not be obtained; And adopt various mixing equipment to stir the rubber powder of caking, due to the snappiness of the thing self that lumps, also be difficult to completely broken, this directly affects the dispersion of waste fluorine rubber powder in viton mixing process, also greatly reduces the loading level of waste rubber powder in rubber unvulcanizate.
When adopting nano inorganic powder to carry out physically encapsulation process to waste fluorine rubber powder surface, because the yardstick of nano inoganic particle is little, in mixing process, be easy to the groove of the uneven surface entering waste fluorine rubber powder, thus inhibit the bonding between rubber powder particle and caking.Wrap up the fluorine rubber powder of process through surface, can place for a long time in packing bag and nothing obviously caking, and when the rubber unvulcanizate adding viton as filler, disperse easily and loading level can be improved significantly.Through the waste fluorine rubber powder of surface modified, when adding rubber unvulcanizate as filler, the nano inorganic material on its surface is few due to content, and under the powerful shear action of mixing process, easily enters the matrix of rubber unvulcanizate, can not cause detrimentally affect to the performance of final product.By controlling the consumption of nano inorganic powder, and selecting mixing equipment and mixing time, the controlled modification to waste fluorine rubber powder surface can be realized, and solve the agglomeration problems of rubber powder.
The test of waste fluorine rubber powder degree of agglomeration: waste fluorine rubber powder is put into plastics bag, the load much larger than rubber powder own wt is placed afterwards above, load is taken off in the specified time, rubber powder in bag is poured into stainless steel steel sieve, sieve, and the material that sieves is weighed, calculate sieving rate, with the degree of the caking of this quantitative evaluation fluorine rubber powder, sieving rate is higher, and degree of agglomeration is lower.
Compared with the technology that the present invention and existing rubber powder directly pack storage, there is positively effect and advance significantly:
(1) the present invention is by carrying out physically encapsulation to the surface of waste fluorine rubber powder, inhibit the caking phenomenon of rubber powder, make rubber powder after storing, still keep high dispersion state, thus ensure that degree of scatter and the high filler loading capacity of rubber powder when adding in rubber unvulcanizate; Through the rubber powder stored, do not need the process again carrying out shredding unit before using, can directly use.
(2) the method is simple, and the finishing degree of waste fluorine rubber powder is controlled, and gives feasibility of batch preparation.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram sheet of surface topography of the inventive method waste fluorine rubber powder without the process of surface physics parcel used.
Fig. 2 is the scanning electron microscope diagram sheet wrapping up the surface topography of the waste fluorine rubber powder of process through surface physics prepared by the inventive method.
Embodiment
Embodiment 1:
A preparation method for the waste fluorine rubber powder of polymolecularity, comprises following order step:
(1) get 100 grams of ambient ground, grinding and cross the waste fluorine rubber powder of 80 mesh sieves, add 5 grams of precipitated silicas, it mixed 5 minutes in high-speed mixer, namely obtain the waste fluorine rubber powder of polymolecularity; In order to examine the degree of agglomeration of rubber powder in storage process, carry out the test under follow-up rigor condition;
(2) powder through the process of surface physics parcel is taken out from mixing tank, load in plastics bag, the rubber powder in bag is pushed into size and is about 100*100mm 2rectangle bulk pile up thing; Then, plastics bag is placed the load of 5000 grams, after leaving standstill 96 hours, removes the load on plastics bag, open plastics bag, materials inside is poured out gently;
(3) by sieved for the rubber powder steel that press through through overload sieve process, to no longer including particle passes through, to sieving, rubber powder is weighed, and calculates sieving rate, and evaluates the solution degree of surperficial physically encapsulation process for agglomeration problems with this; Sieving rate is higher, and degree of agglomeration is lower.
Test result is as following table.
Other embodiment:
Preparation technology is the same.
Remarks: 80 orders processed without surface parcel and 100 object waste fluorine rubber powder are through same loading, unloading and screening, and sieving rate is 37.18% and 28.02% respectively.

Claims (5)

1. a preparation method for the waste fluorine rubber powder of polymolecularity, comprises following order step:
(1) with sieve, the waste fluorine rubber powder that ambient ground, grinding obtain is separated, obtains the rubber powder of different-grain diameter;
(2) waste fluorine rubber powder is loaded in mixing equipment, add nano inorganic powder afterwards, realized the physically encapsulation process of vulcanized rubber powder by mixing; Nano inorganic powder is any one or its arbitrary combination in precipitated silica, nano titanium oxide, nano zine oxide, nano-calcium carbonate;
(3) take out in surface treated waste fluorine rubber powder slave unit, load in bag and store.
2. the preparation method of the waste fluorine rubber powder of a kind of polymolecularity according to claim 1, is characterized in that: described mixing equipment is air driven mixer, drum mixer, double-cone mixer, kneader or high-speed mixer.
3. the preparation method of the waste fluorine rubber powder of a kind of polymolecularity according to claim 1, is characterized in that: the consumption of nano inorganic powder is 3 ~ 8% of waste fluorine rubber powder quality.
4. the preparation method of the waste fluorine rubber powder of a kind of polymolecularity according to claim 1, is characterized in that: waste fluorine rubber powder and nano inorganic powder be blended in normal temperature condition under carry out.
5. the preparation method of the waste fluorine rubber powder of a kind of polymolecularity according to claim 1, is characterized in that: the mixing time adopting high-speed mixer is 5 ~ 10 minutes; The mixing time adopting air driven mixer, drum mixer, double-cone mixer or kneader is 10 ~ 20 minutes.
CN201310553672.0A 2013-11-08 2013-11-08 A kind of preparation method of waste fluorine rubber powder of polymolecularity Expired - Fee Related CN103554519B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1483763A (en) * 2002-09-16 2004-03-24 鲍振林 Modified composition of waste plastics and flyash
CN1517388A (en) * 2003-01-14 2004-08-04 北京泛洋伟业科技有限公司 Process for preparing fine rubber powder from waste rubber by normal temp assistan method
CN101407595A (en) * 2008-11-23 2009-04-15 江西亚中橡塑有限公司 Production method of fine rubber powder and fine rubber powder produced thereby

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6864310B2 (en) * 1999-04-01 2005-03-08 Pirelli Pneumatici S.P.A. Process for manufacturing a tire compound

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1483763A (en) * 2002-09-16 2004-03-24 鲍振林 Modified composition of waste plastics and flyash
CN1517388A (en) * 2003-01-14 2004-08-04 北京泛洋伟业科技有限公司 Process for preparing fine rubber powder from waste rubber by normal temp assistan method
CN101407595A (en) * 2008-11-23 2009-04-15 江西亚中橡塑有限公司 Production method of fine rubber powder and fine rubber powder produced thereby

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