CN104651943B - A kind of barium sulfate crystal whisker and preparation method thereof - Google Patents
A kind of barium sulfate crystal whisker and preparation method thereof Download PDFInfo
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- CN104651943B CN104651943B CN201510034577.9A CN201510034577A CN104651943B CN 104651943 B CN104651943 B CN 104651943B CN 201510034577 A CN201510034577 A CN 201510034577A CN 104651943 B CN104651943 B CN 104651943B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
- C30B30/02—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using electric fields, e.g. electrolysis
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- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a kind of barium sulfate crystal whisker and preparation method thereof, it is especially the influence that the present invention is grown up using electric field and chemical additives to Barium sulfate crystals, prepare a kind of barium sulfate crystal whisker, the barium sulfate crystal whisker not only has excellent weatherability and ageing resistance, and the wearability and impact strength of product can be increased, the toughness of product is significantly improved, and preparation method is simple, cost is cheap, is easy to industrialized production.
Description
Technical field
The invention belongs to chemical material field, is related to field of inorganic nonmetallic material, mainly a kind of barium sulfate crystal whisker and
Its preparation method.
Background technology
Barium sulfate is one of most important inorganic chemical product now, in sector applications such as rubber, plastics, coating, medicine
Extensively, oil, the heavy weight additive of natural gas drilling mud are also used for.Traditional barium sulfate is white rhomboidal crystal, is used as and fills out mostly
Material is added in rubber, plastic products, can strengthen the ageing resistace and weatherability of product, product is non-aging to become fragile, and energy
Surface smoothness is significantly improved, reduces and makes production cost.
With the development of inorganic non-metallic material technology, the barium sulfate of single shape be difficult adapt to and meet market development and
The needs of production, barium sulfate towards diversification, become more meticulous, specialized direction it is fast-developing, thus, barium sulfate is just towards abnormity
Structural development, the barium sulfate of the polymorphic structure such as threadiness, sheet, spherical, hollow, porous is due to its special structure and property
It can be made to assign product special performance in applying.Barium sulfate crystal whisker has more excellent power compared with traditional barium sulfate
Performance is learned, there is the function that toughness reinforcing strengthens to rubber, plastic products.
China Patent Publication No. CN102689916A discloses a kind of liquid phase preparation process of barium sulfate porous microsphere, the hair
The barium sulfate of bright preparation is monocline crystalline phase barium sulfate microballoon, is loose structure or hollow-core construction, and pattern is easily controlled, and compares surface
Product is big, but is unsuitable for toughness reinforcing enhancing of the barium sulfate for increasing rubber, plastic products.
China Patent Publication No. CN102219250A discloses a kind of preparation method of nanometer barium sulfate grains, party's legal system
Standby barium sulfate is nanometer spherical particle, and cost of material is low, and production capacity is big, is also unsuitable for being used to the barium sulfate increase rubber
The toughness and intensity of glue, plastic products.
China Patent Publication No. CN102674428A discloses a kind of high whiteness spherical nano barium sulfate and preparation method thereof,
The barium sulfate that this method is prepared is nanometer spherical barium sulfate, is equally unsuitable for using the barium sulfate as rubber, plastic products
Toughness reinforcing reinforcing material.
According to above-mentioned, the barium sulfate prepared at present using distinct methods is mostly graininess or spherical, because its shape is unfavorable
Scattered in stress causes interiors of products discontinuity, easy fracture or opening, thus is not suitable for as rubber, plastics system
Product toughness reinforcing reinforcing material is added in product, and use range is restricted, so as to limit barium sulfate in rubber, filling plastic
Application.
The content of the invention
Be mostly graininess or spherical for the barium sulfate prepared at present using distinct methods, be not suitable for as rubber,
The defects of plastic products toughness reinforcing reinforcing material is added in product, and use range is restricted propose a kind of barium sulfate crystal whisker and
Its preparation method, to achieve the above object, the influence that the present invention is grown up using electric field and chemical additives to Barium sulfate crystals, system
For a kind of barium sulfate crystal whisker is gone out, the barium sulfate crystal whisker not only has excellent weatherability and ageing resistance, and can increase product
Wearability and impact strength, significantly improve the toughness of product, and preparation method is simple, cost is cheap, is easy to industrial metaplasia
Production.
A kind of barium sulfate crystal whisker of the present invention, it is characterised in that Barium sulfate crystals are grown up using electric field and chemical additives
The barium sulfate with loose fibre structure slightly staggeredly for influenceing to prepare, draw ratio are 10~200: 1.
A kind of preparation method of barium sulfate crystal whisker of the present invention, it is characterised in that using parallel electric field and chemical additives as hand
Section, makes sulfuric acid with electric field line travel motion and chemical additives using charged particle in parallel electric field to the activation of crystal face
Barium carries out crystalline growth along parallel electric field line, obtains a kind of barium sulfate crystal whisker, its specific preparation process is as follows：
1) distilled water of 300-500 parts by weight is added in reaction tank, adds the crystal formation control of 20-30 parts by weight
Agent, and 60-75 DEG C is heated to, after its dissolving, reaction tank is inserted in parallel electric field；
2）Keep temperature and the electric-field intensity of step 1) constant, be 30- by the substance withdrawl syndrome of 15-25 parts by weight
50mmol/L barium source solution and the substance withdrawl syndrome of 15-25 parts by weight are 30-50mmol/L sulfate liquors with 0.2-0.5
The reaction tank both ends of the positive pole from electric field and negative pole add the speed of parts by weight/minute simultaneously respectively, stop adding after reacting 1-2h
Heat, Temperature fall, electric field keep constant, stand 5-7h；
3）By step 2）Obtained solution is filtered, and barium sulfate crystal whisker precipitation is obtained, by its temperature at 100-200 DEG C
Lower vacuum drying 0.5-1h, obtains barium sulfate crystal whisker.
In a kind of specific preparation process of barium sulfate crystal whisker, step 1）Described in chemical additives be ammonium citrate.
In a kind of specific preparation process of barium sulfate crystal whisker, step 1）Described in parallel electric field intensity be 5-20N/C.
In a kind of specific preparation process of barium sulfate crystal whisker, step 2）Described in barium source solution be substance withdrawl syndrome
For one kind in 30-50mmol/L barium chloride, barium hydroxide solution.
In a kind of specific preparation process of barium sulfate crystal whisker, step 2）Described in sulfate liquor be material amount it is dense
The one kind spent in the sodium sulphate, potassium sulfate, ammonium sulfate for 30-50mmol/L.
The principle that the present invention can be migrated with the direction of electric field line in the electric field using charged particle, by barium ions and sulfuric acid
Radical ion respectively from the positive and negative electrodes in same of electric field when add, in the presence of electric field force, barium ions moves along electric field line to negative pole,
Sulfate ion moves along electric field line to positive pole, collide in the process and react generation barium sulfate, due to barium sulfate
Not soluble in water, crystallization separates out, and forms crystal；And the ammonium citrate in solution is easier to act on barium sulfate in the presence of electric field
Crystal is along two faces in electric field line direction, therefore the two faces have higher activity, can adsorb more barium sulfate and fast
Fast-growing is grown, and forms the whisker of threadiness；Again by filtering and drying, barium sulfate crystal whisker is obtained, the barium sulfate crystal whisker not only has
Excellent weatherability and ageing resistance, and the wearability and impact strength of product can be increased, the toughness of product is significantly improved,
And the preparation method is simple, low production cost is easy to operate, is easy to industrialized production.
The characteristics of present invention is prominent and beneficial effect are：
1st, barium sulfate crystal whisker of the present invention is that the influence grown up using electric field and chemical additives to Barium sulfate crystals is prepared
Have slightly staggeredly loose fibre structure barium sulfate, draw ratio be 10~200: 1.
2nd, barium sulfate crystal whisker of the present invention not only has excellent weatherability and ageing resistance, and can increase the wear-resisting of product
Property and impact strength, significantly improve the toughness of product.
3rd, preparation method of the present invention is simple, and low production cost is easy to operate, is easy to industrialized production.
Barium sulfate crystal whisker of the present invention and common barium sulfate performance comparison：Examination criteria is GB1040-92, GB/T 1843-
2008, matrix resin PS；
| Product | Shape | 10% addition impact strength | 10% addition tensile strength | 10% addition elongation at break |
| Common barium sulfate | Graininess is spherical | 4–7 kJ/m2 | 40–50MPa | 3–4% |
| Barium sulfate crystal whisker | Threadiness | 10-15 kJ/m2 | 60-75MPa | 8-12% |
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
1) distilled water of 300 parts by weight is added in reaction tank, adds the ammonium citrate of 20 parts by weight, and be heated to
60 DEG C, after its dissolving, reaction tank is inserted into intensity as in 5N/C parallel electric fields；
2）Keep temperature and the electric-field intensity of step 1) constant, be 30mmol/L's by the substance withdrawl syndrome of 15 parts by weight
Barium chloride solution and the substance withdrawl syndrome of 15 parts by weight are 30mmol/L metabisulfite solution with the speed of 0.5 parts by weight/minute
The reaction tank both ends of the positive pole from electric field and negative pole add degree simultaneously respectively, stop heating, Temperature fall after reacting 1h, electric field is protected
Hold constant, standing 5h；
3）By step 2）Obtained solution is filtered, and obtains barium sulfate crystal whisker precipitation, by its at a temperature of 100 DEG C it is true
Sky dries 0.5h, obtains barium sulfate crystal whisker.
Embodiment 2
1) distilled water of 500 parts by weight is added in reaction tank, adds the ammonium citrate of 30 parts by weight, and be heated to
75 DEG C, after its dissolving, reaction tank is inserted into intensity as in 10N/C parallel electric fields；
2）Keep temperature and the electric-field intensity of step 1) constant, be 50mmol/L's by the substance withdrawl syndrome of 25 parts by weight
Barium hydroxide solution and the substance withdrawl syndrome of 25 parts by weight are 50mmol/L potassium sulfate solution with 0.2 parts by weight/minute
The reaction tank both ends of the positive pole from electric field and negative pole add speed simultaneously respectively, stop heating, Temperature fall, electric field after reacting 2h
Keep constant, stand 7h；
3）By step 2）Obtained solution is filtered, and obtains barium sulfate crystal whisker precipitation, by its at a temperature of 200 DEG C it is true
Sky dries 1h, obtains barium sulfate crystal whisker.
Embodiment 3
1) distilled water of 400 parts by weight is added in reaction tank, adds the ammonium citrate of 25 parts by weight, and be heated to
65 DEG C, after its dissolving, reaction tank is inserted into intensity as in 20N/C parallel electric fields；
2）Keep temperature and the electric-field intensity of step 1) constant, be 40mmol/L's by the substance withdrawl syndrome of 20 parts by weight
Barium chloride solution and the substance withdrawl syndrome of 20 parts by weight are 40mmol/L ammonium sulfate with the speed of 0.3 parts by weight/minute
The reaction tank both ends of the positive pole from electric field and negative pole add degree simultaneously respectively, stop heating, Temperature fall, electric field after reacting 1.5h
Keep constant, stand 6h；
3）By step 2）Obtained solution is filtered, and obtains barium sulfate crystal whisker precipitation, by its at a temperature of 150 DEG C it is true
Sky dries 0.5h, obtains barium sulfate crystal whisker.
Embodiment 4
1) distilled water of 450 parts by weight is added in reaction tank, adds the ammonium citrate of 25 parts by weight, and be heated to
69 DEG C, after its dissolving, reaction tank is inserted into intensity as in 18N/C parallel electric fields；
2）Keep temperature and the electric-field intensity of step 1) constant, be 45mmol/L's by the substance withdrawl syndrome of 25 parts by weight
Barium chloride solution and the substance withdrawl syndrome of 25 parts by weight are 45mmol/L metabisulfite solution with the speed of 0.4 parts by weight/minute
The reaction tank both ends of the positive pole from electric field and negative pole add degree simultaneously respectively, stop heating, Temperature fall, electric field after reacting 1.5h
Keep constant, stand 6.5h；
3）By step 2）Obtained solution is filtered, and obtains barium sulfate crystal whisker precipitation, by its at a temperature of 160 DEG C it is true
Sky dries 0.5h, obtains barium sulfate crystal whisker.
Embodiment 5
1) distilled water of 350 parts by weight is added in reaction tank, adds the ammonium citrate of 25 parts by weight, and be heated to
70 DEG C, after its dissolving, reaction tank is inserted into intensity as in 10N/C parallel electric fields；
2）Keep temperature and the electric-field intensity of step 1) constant, be 35mmol/L's by the substance withdrawl syndrome of 15 parts by weight
Barium hydroxide solution and the substance withdrawl syndrome of 15 parts by weight are 35mmol/L potassium sulfate solution with 0.2 parts by weight/minute
The reaction tank both ends of the positive pole from electric field and negative pole add speed simultaneously respectively, stop heating, Temperature fall, electric field after reacting 2h
Keep constant, stand 5.5h；
3）By step 2）Obtained solution is filtered, and obtains barium sulfate crystal whisker precipitation, by its at a temperature of 180 DEG C it is true
Sky dries 1h, obtains barium sulfate crystal whisker.
Claims (4)
1. a kind of preparation method of barium sulfate crystal whisker, it is characterised in that using parallel electric field and chemical additives as means, using flat
Activation of the charged particle with electric field line travel motion and chemical additives to crystal face in row electric field, make barium sulfate along parallel
Electric field line carries out crystalline growth, obtains a kind of barium sulfate crystal whisker, its specific preparation process is as follows：
1) distilled water of 300-500 parts by weight is added in reaction tank, adds the chemical additives of 20-30 parts by weight, and
60-75 DEG C is heated to, after its dissolving, reaction tank is inserted in parallel electric field；Wherein, described chemical additives are citric acid
Ammonium；
2）Keep temperature and the electric-field intensity of step 1) constant, be 30-50mmol/ by the substance withdrawl syndrome of 15-25 parts by weight
L barium source solution and the substance withdrawl syndrome of 15-25 parts by weight are 30-50mmol/L sulfate liquors with 0.2-0.5 weight
The reaction tank both ends of the positive pole from electric field and negative pole add the speed of part/minute simultaneously respectively, stop heating after reacting 1-2h,
Temperature fall, electric field keep constant, stand 5-7h；
3）By step 2）Obtained solution is filtered, and obtains barium sulfate crystal whisker precipitation, by its at a temperature of 100-200 DEG C it is true
Sky dries 0.5-1h, obtains barium sulfate crystal whisker.
A kind of 2. preparation method of barium sulfate crystal whisker according to claim 1, it is characterised in that described parallel electric field intensity
For 5-20N/C.
3. a kind of preparation method of barium sulfate crystal whisker according to claim 1, it is characterised in that described barium source solution is thing
The amount concentration of matter is one kind in 30-50mmol/L barium chloride, barium hydroxide solution.
4. a kind of preparation method of barium sulfate crystal whisker according to claim 1, it is characterised in that described sulfate liquor is
One kind in sodium sulphate, potassium sulfate, ammonium sulfate that substance withdrawl syndrome is 30-50mmol/L.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510034577.9A CN104651943B (en) | 2015-01-23 | 2015-01-23 | A kind of barium sulfate crystal whisker and preparation method thereof |
| PCT/CN2015/099775 WO2016115966A1 (en) | 2015-01-23 | 2015-12-30 | Barium sulfate whisker and preparation method therefor |
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| CN201510034577.9A CN104651943B (en) | 2015-01-23 | 2015-01-23 | A kind of barium sulfate crystal whisker and preparation method thereof |
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| CN104651943B true CN104651943B (en) | 2017-12-12 |
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| CN104651943B (en) * | 2015-01-23 | 2017-12-12 | 江苏锡沂高新区科技发展有限公司 | A kind of barium sulfate crystal whisker and preparation method thereof |
Citations (3)
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|---|---|---|---|---|
| JP2001020166A (en) * | 1999-07-08 | 2001-01-23 | Japan Vilene Co Ltd | Thermoadhesive whisker, its production, assembly using the same, and production of the assembly |
| CN102827419A (en) * | 2011-06-14 | 2012-12-19 | 黑龙江鑫达企业集团有限公司 | Preparation method for easy-to-disperse and easy-to-process polypropylene composite material |
| CN103320867A (en) * | 2013-04-12 | 2013-09-25 | 武汉理工大学 | Method for electric field assisted preparation of one-dimensional nanometer ZnO crystal whisker |
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| CN101865227B (en) * | 2009-08-25 | 2012-09-05 | 青岛华瑞丰机械有限公司 | Method for preparing brake pad by barium sulfate crystal whisker |
| CN102277061A (en) * | 2011-06-30 | 2011-12-14 | 上海工程技术大学 | Powder coating containing nanowhisker materials and preparation method thereof |
| WO2014179931A1 (en) * | 2013-05-07 | 2014-11-13 | 上海宜瓷龙新材料科技有限公司 | Non-stick coating with antioxidation function, and preparation method therefor |
| CN103628124A (en) * | 2013-11-12 | 2014-03-12 | 西安交通大学 | Low-voltage direct-current electrolysis preparation method of calcium carbonate whisker |
| CN103881418B (en) * | 2014-03-05 | 2016-04-06 | 苏州克莱明新材料有限公司 | The preparation of modified nano-barium sulfate and application thereof |
| CN104195589B (en) * | 2014-08-21 | 2016-05-11 | 成都新柯力化工科技有限公司 | A kind of preparation method of nano barium sulfate and application |
| CN104651943B (en) * | 2015-01-23 | 2017-12-12 | 江苏锡沂高新区科技发展有限公司 | A kind of barium sulfate crystal whisker and preparation method thereof |
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- 2015-01-23 CN CN201510034577.9A patent/CN104651943B/en active Active
- 2015-12-30 WO PCT/CN2015/099775 patent/WO2016115966A1/en active Application Filing
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|---|---|---|---|---|
| JP2001020166A (en) * | 1999-07-08 | 2001-01-23 | Japan Vilene Co Ltd | Thermoadhesive whisker, its production, assembly using the same, and production of the assembly |
| CN102827419A (en) * | 2011-06-14 | 2012-12-19 | 黑龙江鑫达企业集团有限公司 | Preparation method for easy-to-disperse and easy-to-process polypropylene composite material |
| CN103320867A (en) * | 2013-04-12 | 2013-09-25 | 武汉理工大学 | Method for electric field assisted preparation of one-dimensional nanometer ZnO crystal whisker |
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| Title |
|---|
| Formation of BaSO4 Whiskers in Microemulsion;Shunichi IIDA et al.;《Journal of Chemical Engineering of Japan》;20051231;第38卷(第5期);第357-359页 * |
| Oriented Crystallization of Fresnoite in an Electric Field;Ralf Keding et al.;《Ber. Bunsenges. Phy. Chem.》;19961231;第100卷(第9期);第1515-1518页 * |
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| WO2016115966A1 (en) | 2016-07-28 |
| CN104651943A (en) | 2015-05-27 |
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