CN103435355A - Method for preparing TiCN powder by respectively taking butyl titanate and sucrose as titanium source and carbon source - Google Patents
Method for preparing TiCN powder by respectively taking butyl titanate and sucrose as titanium source and carbon source Download PDFInfo
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- CN103435355A CN103435355A CN201310382991XA CN201310382991A CN103435355A CN 103435355 A CN103435355 A CN 103435355A CN 201310382991X A CN201310382991X A CN 201310382991XA CN 201310382991 A CN201310382991 A CN 201310382991A CN 103435355 A CN103435355 A CN 103435355A
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- sucrose
- powder
- purity
- tetrabutyl titanate
- ticn powder
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- 239000000843 powder Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 24
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 title claims abstract description 14
- 229930006000 Sucrose Natural products 0.000 title claims abstract description 14
- 239000005720 sucrose Substances 0.000 title claims abstract description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 12
- 239000010936 titanium Substances 0.000 title abstract description 12
- 229910052719 titanium Inorganic materials 0.000 title abstract description 12
- 229910052799 carbon Inorganic materials 0.000 title abstract description 9
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 title 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000012047 saturated solution Substances 0.000 claims abstract description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 3
- 238000005516 engineering process Methods 0.000 claims description 7
- 239000013064 chemical raw material Substances 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract 2
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000005121 nitriding Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种以钛酸四丁酯和蔗糖分别为钛源和碳源制备TiCN粉体的方法。将钛酸四丁酯溶于无水乙醇中制得饱和溶液，将蔗糖溶于去离子水中制得饱和溶液；将两种饱和溶液按钛酸四丁酯和蔗糖质量比1:8~12均匀混合，在100~150℃下干燥24~48小时，制得前驱体；所得前驱体在氮气氛或氨分解气氛保护下加热至1300~2000℃，保温1~2小时进行碳热还原和氮化，制得TiCN粉体；所述化学试剂及原料的纯度均为分析纯及以上纯度；所制得粉体的组成由加入原料配比控制，纯度和粒度由加料顺序和制备工艺共同决定。本发明方法具有原料混合均匀、工艺简单、合成温度低、合成时间短以及节能环保等特点。The invention discloses a method for preparing TiCN powder by using tetrabutyl titanate and sucrose as titanium source and carbon source respectively. Dissolve tetrabutyl titanate in absolute ethanol to obtain a saturated solution, and dissolve sucrose in deionized water to obtain a saturated solution; the two saturated solutions are evenly mixed according to the mass ratio of tetrabutyl titanate to sucrose: 1:8~12 Mix and dry at 100-150°C for 24-48 hours to obtain a precursor; the obtained precursor is heated to 1300-2000°C under the protection of a nitrogen atmosphere or an ammonia decomposition atmosphere, and kept for 1-2 hours for carbothermal reduction and nitriding , TiCN powder is obtained; the purity of the chemical reagents and raw materials are analytically pure and above; the composition of the prepared powder is controlled by the ratio of raw materials added, and the purity and particle size are determined by the order of addition and the preparation process. The method of the invention has the characteristics of uniform mixing of raw materials, simple process, low synthesis temperature, short synthesis time, energy saving and environmental protection, and the like.
Description
Technical field
The invention belongs to TiCN Preparation Technique of Powders field, particularly a kind ofly with tetrabutyl titanate and sucrose, be respectively the method that titanium source and carbon source prepare the TiCN powder.
Background technology
TiCN has high-melting-point, high rigidity, high-wearing feature and the special characteristics such as functional, not only be widely used in the reinforcement of grinding tool, cutting tool and matrix material etc., also as energy and material, be used widely, and have a wide range of applications in new function material.
Superfine Ti CN powder is badly in need of in the modern energy industrial development.Tradition TiO
2with the synthetic TiCN powder of high temperature reduction after the carbon solid phase mixing, with low cost but powder preparation is thicker; At present mainly to take pure titanium, titanium organism or gaseous titanium compound be raw material to superfine Ti CN powder, and with the preparation of the techniques such as vapour deposition, plasma heating, raw material and process costs are high, make superfine Ti CN powder expensive.Research and the low-cost preparation of application superfine Ti CN new technology are highly significant.
The TiCN powder that large-scale industrialization is produced at present is mostly 2 ~ 5 μ m, along with the development of modernization industry, and the especially development of energy industry, increasing to the demand of ultrafine powder TiCN, superfine Ti CN has higher using value, has a extensive future.But the superfine Ti CN powder of existing market supply is because raw materials cost and preparation technology's cost are high and expensive.Therefore the research of carrying out low-cost preparation ultrafine powder TiCN has very large realistic meaning.
The preparation of superfine Ti CN powder is the focus of material supply section scholar research, existing raw material aspect, the aspect of research, process aspect is also arranged.But diverse ways has its relative merits for suitability for industrialized production.
Direct carborization is with simple substance carbon, metallic titanium powder (or TiH
2) be raw material, at high temperature, in nitrogen-based atmosphere, the direct contact reacts of reactant generates TiCN, and product purity is high, the carbon metering is than large, and technological process is simple.But titanium valve is expensive, the preparation of purification ultrafine titanium powder is more difficult; Reaction process is difficult to be controlled, and the TiCN synthesized needs further grinding fragmentation, causes the purity drop of product, also will further purify, and makes the standby superfine Ti CN powder of this legal system obtain large-scale promotion.
Carbothermic method is the traditional method of TiCN powder suitability for industrialized production.This technique is with TiO
2for the titanium source, take graphite, carbon black, activated carbon etc. is the C source, under high temperature, nitrogen group protecting atmosphere, and TiO
2generated the TiCN powder by the C reduction.Advantage is: raw materials cost is low; Technique is simple, and production efficiency is higher; The granularity of TiCN is micron order.But raw material is poor by the mechanically mixing homogeneity; TiCN is also easily oxidized.With regard to current production technology, the powder synthesized can not meet the requirement of fine ceramics fully on granularity and purity.
Also have some other method to prepare superfine Ti CN, but generally have the high organic compound as high pure metal titanium valve, titanium of ingredient requirement etc.; The synthesis technique complexity, as need heating plasma, microwave heating, vapour deposition etc., appointed condition requires the problems such as high, and preparation method or complex process or output are limited, cause cost high.Exploitation high-level efficiency, TiCN ultrafine powder technology cheaply, remain the emphasis of countries nowadays scientist and business circles research.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of and be respectively with tetrabutyl titanate and sucrose the method that titanium source and carbon source prepare the TiCN powder.
Concrete steps are:
(1) tetrabutyl titanate is dissolved in dehydrated alcohol and makes saturated solution, sucrose is dissolved in deionized water and makes saturated solution.
(2) two kinds of saturated solutions that step (1) made evenly mix by tetrabutyl titanate and sucrose mass ratio 1:8 ~ 12, and gained mixed solution under 100 ~ 150 ℃ dry 24 ~ 48 hours, make presoma.
(3) presoma step (2) made is heated to 1300 ~ 2000 ℃ under nitrogen atmosphere or ammonia dissolving atmosphere protection, is incubated 1 ~ 2 hour and carries out carbothermic reduction and nitrogenize, makes the TiCN powder.
The purity of described chemical reagent and raw material is analytical pure and above purity.
The composition of the prepared TiCN powder of the present invention is by adding proportioning raw materials to control, and the purity of powder and granularity are determined jointly by order of addition(of ingredients) and preparation technology.
The advantage of the inventive method:
(1) take sucrose as carbon source, take tetrabutyl titanate as the titanium source, through carbothermic reduction, high-purity, the superfine Ti CN of low-cost preparation.
(2) method for preparing TiCN with tradition is compared, and has that raw material mixes, technique is simple, synthesis temperature is low, generated time is short and the characteristics such as energy-conserving and environment-protective.
embodiment
embodiment:
(1) tetrabutyl titanate is dissolved in dehydrated alcohol and makes saturated solution, sucrose is dissolved in deionized water and makes saturated solution.
(2) two kinds of saturated solutions that step (1) made evenly mix by tetrabutyl titanate and sucrose mass ratio 1:10, and gained mixed solution under 130 ℃ dry 34 hours, make presoma.
(3) presoma step (2) made is heated to 1850 ℃ under the ammonia dissolving atmosphere protection; be incubated and within 1 hour 40 minutes, carry out carbothermic reduction and nitrogenize; make the TiCN powder, gained TiCN powder is the superfine Ti CN powder that particle diameter is 150 ~ 300 nanometers through the testing graininess analysis.
The purity of described chemical reagent and raw material is analytical pure.
Claims (2)
1. a method for preparing the TiCN powder is characterized in that concrete steps are:
(1) tetrabutyl titanate is dissolved in dehydrated alcohol and makes saturated solution, sucrose is dissolved in deionized water and makes saturated solution;
(2) two kinds of saturated solutions that step (1) made evenly mix by tetrabutyl titanate and sucrose mass ratio 1:8 ~ 12, and gained mixed solution under 100 ~ 150 ℃ dry 24 ~ 48 hours, make presoma;
(3) presoma step (2) made is heated to 1300 ~ 2000 ℃ under nitrogen atmosphere or ammonia dissolving atmosphere protection, is incubated 1 ~ 2 hour and carries out carbothermic reduction and nitrogenize, makes the TiCN powder;
The purity of described chemical reagent and raw material is analytical pure and above purity.
2. the method for preparing the TiCN powder according to claim 1 is characterized in that: the composition of prepared TiCN powder is controlled by the proportioning that adds raw material, and the purity of powder and granularity are determined jointly by order of addition(of ingredients) and preparation technology.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310382991XA CN103435355A (en) | 2013-08-28 | 2013-08-28 | Method for preparing TiCN powder by respectively taking butyl titanate and sucrose as titanium source and carbon source |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310382991XA CN103435355A (en) | 2013-08-28 | 2013-08-28 | Method for preparing TiCN powder by respectively taking butyl titanate and sucrose as titanium source and carbon source |
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| Publication Number | Publication Date |
|---|---|
| CN103435355A true CN103435355A (en) | 2013-12-11 |
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| CN201310382991XA Pending CN103435355A (en) | 2013-08-28 | 2013-08-28 | Method for preparing TiCN powder by respectively taking butyl titanate and sucrose as titanium source and carbon source |
Country Status (1)
| Country | Link |
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| CN (1) | CN103435355A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486462A (en) * | 2009-02-23 | 2009-07-22 | 潍坊学院 | Preparation of titanium carbide micro powder |
| CN102583376A (en) * | 2012-03-15 | 2012-07-18 | 株洲精工硬质合金有限公司 | Nano titanium carbide (TiC) powder and preparation method and application thereof |
| CN103130506A (en) * | 2013-03-15 | 2013-06-05 | 长沙伟徽高科技新材料股份有限公司 | Method for preparing superfine titanium carbonitride |
-
2013
- 2013-08-28 CN CN201310382991XA patent/CN103435355A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486462A (en) * | 2009-02-23 | 2009-07-22 | 潍坊学院 | Preparation of titanium carbide micro powder |
| CN102583376A (en) * | 2012-03-15 | 2012-07-18 | 株洲精工硬质合金有限公司 | Nano titanium carbide (TiC) powder and preparation method and application thereof |
| CN103130506A (en) * | 2013-03-15 | 2013-06-05 | 长沙伟徽高科技新材料股份有限公司 | Method for preparing superfine titanium carbonitride |
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| PB01 | Publication | ||
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Application publication date: 20131211 |