CN104651943A - Barium sulfate whisker and preparation method thereof - Google Patents
Barium sulfate whisker and preparation method thereof Download PDFInfo
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- CN104651943A CN104651943A CN201510034577.9A CN201510034577A CN104651943A CN 104651943 A CN104651943 A CN 104651943A CN 201510034577 A CN201510034577 A CN 201510034577A CN 104651943 A CN104651943 A CN 104651943A
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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
- 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
- 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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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a barium sulfate whisker and a preparation method of the barium sulfate whisker. The barium sulfate whisker is prepared by utilizing the influence on the growth of the barium sulfate whisker by an electric field and a crystal form controlling agent. The barium sulfate whisker is high in weather resistance and anti-aging property; moreover, the abrasion property and the anti-impact strength of the product can be increased, and the toughness of the product is obviously improved; the preparation method is simple, low in cost and easy for industrial production.
Description
Technical field
The invention belongs to chemical material field, relate to field of inorganic nonmetallic material, mainly a kind of barium sulfate crystal whisker and preparation method thereof.
Background technology
Barium sulfate is one of most important inorganic chemical product now, extensive in sector applications such as rubber, plastics, coating, medicine, also for the weighting agent of oil, Sweet natural gas drilling mud.Traditional barium sulfate is white rhomboidal crystal, mostly joins in rubber, plastics as filler, can strengthen ageing resistance and the weathering resistance of product, and product is not easily aging to become fragile, and significantly can improve surface smoothness, reduces and makes production cost.
Along with the development of ceramic technology, the barium sulfate of single shape is difficult to the needs adapting to and meet market development and production, barium sulfate towards diversification, become more meticulous, specialized direction is fast-developing, thus, barium sulfate just towards polymorphic structure development, the barium sulfate of the polymorphic structures such as such as threadiness, sheet, spherical, hollow, porous due to its special stuctures and properties make it apply in give product special performance.Barium sulfate crystal whisker, compared with traditional barium sulfate, has more excellent mechanical property, rubber, plastics is had to the function of toughen and intensify.
China Patent Publication No. CN102689916A discloses a kind of liquid phase preparation process of barium sulfate porous microsphere, barium sulfate prepared by this invention is monocline crystalline phase barium sulfate microballoon, for vesicular structure or hollow structure, and pattern easily controls, specific surface area is large, but is unsuitable for the toughen and intensify of this barium sulfate for increasing rubber, plastics.
China Patent Publication No. CN102219250A discloses a kind of preparation method of nanometer barium sulfate grains, barium sulfate prepared by the method is nanometer spherical particle, raw materials cost is low, and throughput is large, is also unsuitable for this barium sulfate for increasing the toughness of rubber, plastics and intensity.
China Patent Publication No. CN102674428A discloses a kind of high whiteness spherical nano barium sulfate and preparation method thereof, the barium sulfate that the method prepares is nanometer spherical barium sulfate, is unsuitable for the toughen and intensify material of this barium sulfate as rubber, plastics equally.
According to above-mentioned, barium sulfate prepared by current employing different methods mostly is particulate state or spherical, because its shape is unfavorable for that the dispersion of stress causes interiors of products discontinuity, easy fracture or opening, thus be not all suitable for and add in product as rubber, plastics toughen and intensify material, use range is restricted, thus limits the application of barium sulfate in rubber, filling plastic.
Summary of the invention
Particulate state or spherical mostly is for the barium sulfate adopting different methods to prepare at present, all be not suitable for as rubber, plastics toughen and intensify material adds in product, the defect that use range is restricted proposes a kind of barium sulfate crystal whisker and preparation method thereof, for achieving the above object, the impact that the present invention utilizes electric field and chemical additives to grow up on Barium sulfate crystals, prepare a kind of barium sulfate crystal whisker, this barium sulfate crystal whisker not only has excellent weathering resistance and resistance to deterioration, and wear resistance and the resistance to impact shock of goods can be increased, significantly improve the toughness of goods, and preparation method is simple, with low cost, be easy to suitability for industrialized production.
A kind of barium sulfate crystal whisker of the present invention, it is characterized in that the barium sulfate with slight staggered loose fibrous texture utilizing electric field and chemical additives to prepare the impact that Barium sulfate crystals is grown up, length-to-diameter ratio is 10 ~ 200: 1.
The preparation method of a kind of barium sulfate crystal whisker of the present invention, it is characterized in that with parallel electric field and chemical additives for means, to utilize in parallel electric field charged particle with electric field line locomotory movement and chemical additives to the activation of crystal face, barium sulfate is made to carry out crystalline growth along parallel electric field line, obtain a kind of barium sulfate crystal whisker, its concrete preparation process is as follows:
1) distilled water of 300-500 weight part is joined in reaction tank, then add the whisker control agent of 20-30 weight part, and be heated to 60-75 DEG C, after it dissolves, reaction tank is inserted in parallel electric field;
2) keep step 1) temperature and strength of electric field constant, to be the barium source solution of 30-50mmol/L and the substance withdrawl syndrome of 15-25 weight part by the substance withdrawl syndrome of 15-25 weight part be 30-50mmol/L sulfate liquor with 0.2-0.5 weight part/minute speed add from the reaction tank two ends of the positive pole of electric field and negative pole respectively simultaneously, heating is stopped after reaction 1-2h, Temperature fall, electric field remains unchanged, and leaves standstill 5-7h;
3) by step 2) solution that obtains filters, obtains barium sulfate crystal whisker precipitation, by its vacuum-drying 0.5-1h at the temperature of 100-200 DEG C, obtain barium sulfate crystal whisker.
In a kind of concrete preparation process of barium sulfate crystal whisker, the chemical additives described in step 1) is ammonium citrate.
In a kind of concrete preparation process of barium sulfate crystal whisker, the parallel electric field intensity described in step 1) is 5-20N/C.
In a kind of concrete preparation process of barium sulfate crystal whisker, step 2) described in the bariumchloride of barium source solution to be substance withdrawl syndrome be 30-50mmol/L, one in barium hydroxide solution.
In a kind of concrete preparation process of barium sulfate crystal whisker, step 2) described in the sodium sulfate of sulfate liquor to be substance withdrawl syndrome be 30-50mmol/L, potassium sulfate, one in ammoniumsulphate soln.
The principle that the present invention utilizes charged particle can move along with the direction of electric field line in the electric field, barium ion and sulfate ion are added from during the positive and negative electrodes in same of electric field respectively, under the effect of electrical forces, barium ion moves along electric field line to negative pole, sulfate ion moves along electric field line to positive pole, collides in the process and the generation barium sulfate that reacts, because barium sulfate is water insoluble, crystallization, forms crystal; And the ammonium citrate in solution more easily acts on Barium sulfate crystals along on two faces in electric field line direction under the effect of electric field, therefore these two masks have higher activity, can adsorb more barium sulfate and growth fast, form fibrous whisker; Again by filtering and drying, obtain barium sulfate crystal whisker, this barium sulfate crystal whisker not only has excellent weathering resistance and resistance to deterioration, and wear resistance and the resistance to impact shock of goods can be increased, significantly improve the toughness of goods, and this preparation method is simple, low production cost, easy to operate, be easy to suitability for industrialized production.
The feature that the present invention gives prominence to and beneficial effect are:
1, barium sulfate crystal whisker of the present invention is the barium sulfate with slight staggered loose fibrous texture utilizing electric field and chemical additives to prepare the impact that Barium sulfate crystals is grown up, and length-to-diameter ratio is 10 ~ 200: 1.
2, barium sulfate crystal whisker of the present invention not only has excellent weathering resistance and resistance to deterioration, and can increase wear resistance and the resistance to impact shock of goods, significantly improves the toughness of goods.
3, preparation method of the present invention is simple, and low production cost is easy to operate, is easy to suitability for 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 is PS;
| Product | Shape | 10% adds resistance to impact shock | 10% adds tensile strength | 10% adds elongation at break |
| Common barium sulfate | Particulate state or spherical | 4–7 kJ/m 2 | 40–50MPa | 3–4% |
| Barium sulfate crystal whisker | Threadiness | 10-15 kJ/m 2 | 60-75MPa | 8-12% |
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should be interpreted as scope of the present invention is only limitted to following example.When not departing from aforesaid method thought of the present invention, the various replacement made according to ordinary skill knowledge and customary means or change, all should be within the scope of the present invention.
embodiment 1
1) joined in reaction tank by the distilled water of 300 weight parts, then add the ammonium citrate of 20 weight parts, and be heated to 60 DEG C, after it dissolves, reaction tank being inserted intensity is in 5N/C parallel electric field;
2) keep step 1) temperature and strength of electric field constant, the metabisulfite solution of to be the barium chloride solution of 30mmol/L and the substance withdrawl syndrome of 15 weight parts by the substance withdrawl syndrome of 15 weight parts be 30mmol/L with 0.5 weight part/minute speed add from the reaction tank two ends of the positive pole of electric field and negative pole respectively simultaneously, heating is stopped after reaction 1h, Temperature fall, electric field remains unchanged, and leaves standstill 5h;
3) by step 2) solution that obtains filters, obtains barium sulfate crystal whisker precipitation, by its vacuum-drying 0.5h at the temperature of 100 DEG C, obtain barium sulfate crystal whisker.
embodiment 2
1) joined in reaction tank by the distilled water of 500 weight parts, then add the ammonium citrate of 30 weight parts, and be heated to 75 DEG C, after it dissolves, reaction tank being inserted intensity is in 10N/C parallel electric field;
2) keep step 1) temperature and strength of electric field constant, the potassium sulfate solution of to be the barium hydroxide solution of 50mmol/L and the substance withdrawl syndrome of 25 weight parts by the substance withdrawl syndrome of 25 weight parts be 50mmol/L with 0.2 weight part/minute speed add from the reaction tank two ends of the positive pole of electric field and negative pole respectively simultaneously, heating is stopped after reaction 2h, Temperature fall, electric field remains unchanged, and leaves standstill 7h;
3) by step 2) solution that obtains filters, obtains barium sulfate crystal whisker precipitation, by its vacuum-drying 1h at the temperature of 200 DEG C, obtain barium sulfate crystal whisker.
embodiment 3
1) joined in reaction tank by the distilled water of 400 weight parts, then add the ammonium citrate of 25 weight parts, and be heated to 65 DEG C, after it dissolves, reaction tank being inserted intensity is in 20N/C parallel electric field;
2) keep step 1) temperature and strength of electric field constant, the ammoniumsulphate soln of to be the barium chloride solution of 40mmol/L and the substance withdrawl syndrome of 20 weight parts by the substance withdrawl syndrome of 20 weight parts be 40mmol/L with 0.3 weight part/minute speed add from the reaction tank two ends of the positive pole of electric field and negative pole respectively simultaneously, heating is stopped after reaction 1.5h, Temperature fall, electric field remains unchanged, and leaves standstill 6h;
3) by step 2) solution that obtains filters, obtains barium sulfate crystal whisker precipitation, by its vacuum-drying 0.5h at the temperature of 150 DEG C, obtain barium sulfate crystal whisker.
embodiment 4
1) joined in reaction tank by the distilled water of 450 weight parts, then add the ammonium citrate of 25 weight parts, and be heated to 69 DEG C, after it dissolves, reaction tank being inserted intensity is in 18N/C parallel electric field;
2) keep step 1) temperature and strength of electric field constant, the metabisulfite solution of to be the barium chloride solution of 45mmol/L and the substance withdrawl syndrome of 25 weight parts by the substance withdrawl syndrome of 25 weight parts be 45mmol/L with 0.4 weight part/minute speed add from the reaction tank two ends of the positive pole of electric field and negative pole respectively simultaneously, heating is stopped after reaction 1.5h, Temperature fall, electric field remains unchanged, and leaves standstill 6.5h;
3) by step 2) solution that obtains filters, obtains barium sulfate crystal whisker precipitation, by its vacuum-drying 0.5h at the temperature of 160 DEG C, obtain barium sulfate crystal whisker.
embodiment 5
1) joined in reaction tank by the distilled water of 350 weight parts, then add the ammonium citrate of 25 weight parts, and be heated to 70 DEG C, after it dissolves, reaction tank being inserted intensity is in 10N/C parallel electric field;
2) keep step 1) temperature and strength of electric field constant, the potassium sulfate solution of to be the barium hydroxide solution of 35mmol/L and the substance withdrawl syndrome of 15 weight parts by the substance withdrawl syndrome of 15 weight parts be 35mmol/L with 0.2 weight part/minute speed add from the reaction tank two ends of the positive pole of electric field and negative pole respectively simultaneously, heating is stopped after reaction 2h, Temperature fall, electric field remains unchanged, and leaves standstill 5.5h;
3) by step 2) solution that obtains filters, obtains barium sulfate crystal whisker precipitation, by its vacuum-drying 1h at the temperature of 180 DEG C, obtain barium sulfate crystal whisker.
Claims (6)
1. a barium sulfate crystal whisker, it is characterized in that the barium sulfate with slight staggered loose fibrous texture utilizing electric field and chemical additives to prepare the impact that Barium sulfate crystals is grown up, length-to-diameter ratio is 10 ~ 200: 1.
2. the preparation method of a barium sulfate crystal whisker, it is characterized in that with parallel electric field and chemical additives for means, to utilize in parallel electric field charged particle with electric field line locomotory movement and chemical additives to the activation of crystal face, barium sulfate is made to carry out crystalline growth along parallel electric field line, obtain a kind of barium sulfate crystal whisker, its concrete preparation process is as follows:
1) distilled water of 300-500 weight part is joined in reaction tank, then add the whisker control agent of 20-30 weight part, and be heated to 60-75 DEG C, after it dissolves, reaction tank is inserted in parallel electric field;
2) keep step 1) temperature and strength of electric field constant, to be the barium source solution of 30-50mmol/L and the substance withdrawl syndrome of 15-25 weight part by the substance withdrawl syndrome of 15-25 weight part be 30-50mmol/L sulfate liquor with 0.2-0.5 weight part/minute speed add from the reaction tank two ends of the positive pole of electric field and negative pole respectively simultaneously, heating is stopped after reaction 1-2h, Temperature fall, electric field remains unchanged, and leaves standstill 5-7h;
3) by step 2) solution that obtains filters, obtains barium sulfate crystal whisker precipitation, by its vacuum-drying 0.5-1h at the temperature of 100-200 DEG C, obtain barium sulfate crystal whisker.
3. the preparation method of a kind of barium sulfate crystal whisker according to claim 2, is characterized in that described chemical additives is ammonium citrate.
4. the preparation method of a kind of barium sulfate crystal whisker according to claim 2, is characterized in that described parallel electric field intensity is 5-20N/C.
5. the preparation method of a kind of barium sulfate crystal whisker according to claim 2, is characterized in that described barium source solution to be substance withdrawl syndrome is the one in the bariumchloride of 30-50mmol/L, barium hydroxide solution.
6. the preparation method of a kind of barium sulfate crystal whisker according to claim 2, is characterized in that described sulfate liquor to be substance withdrawl syndrome is the one in the sodium sulfate of 30-50mmol/L, potassium sulfate, ammoniumsulphate soln.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| 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 |
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| CN104651943A true CN104651943A (en) | 2015-05-27 |
| CN104651943B CN104651943B (en) | 2017-12-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016115966A1 (en) * | 2015-01-23 | 2016-07-28 | 成都新柯力化工科技有限公司 | Barium sulfate whisker and preparation method therefor |
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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 |
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| 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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Family Cites Families (5)
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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 |
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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 |
-
2015
- 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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| WO2016115966A1 (en) * | 2015-01-23 | 2016-07-28 | 成都新柯力化工科技有限公司 | Barium sulfate whisker and preparation method therefor |
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| Publication number | Publication date |
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| CN104651943B (en) | 2017-12-12 |
| WO2016115966A1 (en) | 2016-07-28 |
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