CN1443876A - Preparation method of titanium boride cathode material with gradient function of aluminium electrolytic bath - Google Patents

Preparation method of titanium boride cathode material with gradient function of aluminium electrolytic bath Download PDF

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CN1443876A
CN1443876A CN 02107239 CN02107239A CN1443876A CN 1443876 A CN1443876 A CN 1443876A CN 02107239 CN02107239 CN 02107239 CN 02107239 A CN02107239 A CN 02107239A CN 1443876 A CN1443876 A CN 1443876A
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technical pure
powder less
coating
carbon fiber
aluminium electrolytic
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CN1203216C (en
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赖延清
李庆余
李劼
杨建红
肖劲
刘业翔
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Central South University
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Abstract

The present invention relates to a method for preparing TiB2 cathode material with gradient function for aluminium electrolytic tank, and is characterized by that single formula of TiB2 coating of cathode for aluminium electrolytic tank is changed into several formulae, and single-layer one-step coat-brushing method is changed into multi-layer applying method, and in the course of preparation the solidification heating and carbonization heating system can be seriously controlled, so that the deformation of TiB2 coating in the course of carbonizatino can be reduced, and the cohesional strength of the TiB2 coating and cathode carbon lining of aluminium electrolytic tank is raised, and the coating cathode material with good thermal impact resistance can be obtained.

Description

The preparation method of titanium boride cathode material with gradient function of aluminium electrolytic bath
The present invention relates to aluminium electrolytic cell cathode, particularly relate to a kind of aluminum electrolyzing cell used TiB 2The preparation method of cathode material and coating.
The preparation method of existing cathode of aluminium electrolytic bath titanium boride material and coating is with thermosetting resin and powdery TiB 2Be mixed with into coating, single prescription, individual layer is disposable to be painted on the aluminium electrolysis cathode liner, and hot setting, charing are prepared into coating then.TiB in the coating 2Content distribution be uniform.The wettability quality of aluminium liquid and coating depends on TiB in the coating 2Content, have only and work as
Figure A0210723900081
Just can have excellent wetting capacity between aluminium liquid and the coating, the another kind of major ingredients of coating is a carbon after the charing, and the content of carbon is low more, and aluminium liquid reacts with it and generates Al 4C 3, it is just more little that coating is the possibility that powdery drops., the content of carbon is low more, TiB 2Content high more, the thermal expansivity difference of coating and carbon cathode is just big more, thermal shock resistance is just poor, bonding strength between the two is also poor more, coating just is bulk and drops.Improve the ability of bonding strength and heat shock resistance, dwindle the thermal expansivity difference of coating and carbon cathode, just must improve the content of carbon in the coating, reduce TiB 2Content, so, coating can be powdery again and drop, and generates Al with the reaction of aluminium liquid 4C 3Possibility also can become big.
The objective of the invention is to: overcome the weak point of prior art, provide that a kind of thermal shock resistance is good, bonding strength is big, the TiB good with aluminum-liquid wetting 2The cathode of aluminium electrolytic bath preparation methods that content changes in gradient.
The present invention is for achieving the above object, and the technical scheme of employing is: change the single prescription of cathode of aluminium electrolytic bath titanium boride coating into multiple formulations, the disposable squeegee process of individual layer changes the multilayer streak method into, and the TiB of each layer 2Content changes in gradient, and concrete steps are:
One, smears the preparation method of two layers of thickener
(1) smear first coating with the titanium boride thickener of filling a prescription 1. on cathode of aluminium electrolytic bath, it is 25-60 ℃ that temperature increasing schedule is solidified in control: 10 ℃/h; 60-120 ℃: 5 ℃/h; 120-180 ℃: 9 ℃/h; 180-220 ℃: 6 ℃/h; 220-280 ℃: 8 ℃/h;
(2) smear second coating with the titanium boride thickener of filling a prescription 2. on cathode of aluminium electrolytic bath, it is 25-60 ℃ that temperature increasing schedule is solidified in control: 10 ℃/h; 60-120 ℃: 4 ℃/h; 120-180 ℃: 8 ℃/h; 180-210 ℃: 5 ℃/h;
(3) control charing temperature increasing schedule is 25-300 ℃: 25 ℃/h; 300-600 ℃: 8 ℃/h; 600-900 ℃: 12 ℃/h.
Perhaps:
Two, smear the preparation method of three layers of thickener
(4) smear first coating with the titanium boride thickener of filling a prescription 3. on cathode of aluminium electrolytic bath, it is 25-60 ℃ that temperature increasing schedule is solidified in control: 12 ℃/h; 60-120 ℃: 8 ℃/h; 120-180 ℃: 10 ℃/h; 180-220 ℃: 8 ℃/h; 220-300 ℃: 10 ℃/h.
(5) smear second coating with the titanium boride thickener of filling a prescription 4. on cathode of aluminium electrolytic bath, it is 25-60 ℃ that temperature increasing schedule is solidified in control: 9 ℃/h; 60-120 ℃: 5 ℃/h; 120-180 ℃: 9 ℃/h; 180-220 ℃: 6 ℃/h; 220-250 ℃: 7 ℃/h;
(6) smear the 3rd coating with the titanium boride thickener of filling a prescription 5. on cathode of aluminium electrolytic bath, it is 25-60 ℃ that temperature increasing schedule is solidified in control: 10 ℃/h; 60-120 ℃: 4 ℃/h; 120-180 ℃: 8 ℃/h; 180-210 ℃: 5 ℃/h;
(7) control carbonization temperature increasing schedule is 25-300 ℃: 25 ℃/h; 300-600 ℃: 8 ℃/h; 600-900 ℃: 12 ℃/h.
The prescription of two layers of smearing method is shown in table 1,2:
Table 1 the first layer paste formula 1.
Title Specification Weight percentage (%)
TiB 2Powder 3-10μm ????10-30
Petroleum coke powder Less than 147 μ m 147-246 μ m ????15-30 ????5-15
Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????0.5-1
The carbon fiber bar powder Less than 74 μ m ????1-2
Furane resin Viscosity-average molecular weight 4000-6000 ????15-20
Resins, epoxy E-44 ????5-10
The oxidized bitumen powder Less than 147 μ m ????8-15
Ethanol Technical pure ????2-8
Acetone Technical pure ????2-8
Ethyl acetate Technical pure ????1-5
Sulfuric acid acetate Technical pure ????1-3
Phosphoric acid second fat Technical pure ????1-3
Table 2 second layer paste formula 2.
Title Specification Weight percentage (%)
TiB 2Powder 3-10μm ????40-70
Petroleum coke powder Less than 147 μ m 60 less than 147 μ m ????5-15 ????3-8
Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????0.5-1
The carbon fiber bar powder Less than 74 μ m ????1-2
Furane resin Viscosity-average molecular weight 4000-6000 ????10-15
Resins, epoxy E-44 ????3-8
The oxidized bitumen powder Less than 147 μ m ????5-10
Ethanol Technical pure ????2-8
Acetone Technical pure ????2-8
Ethyl acetate Technical pure ????1-5
Sulfuric acid acetate Technical pure ????0.5-2
Phosphoric acid second fat Technical pure ????0.5-2
The prescription of render float and set method such as table 3,4,5:
Table 3 the first layer paste formula 3.
Title Specification Weight percentage (%)
TiB 2Powder 3-10μm ????5-15
Petroleum coke powder Less than 147 μ m 147-246 μ m ????20-40 ????10-20
Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????1-3
The carbon fiber bar powder Less than 74 μ m ????2-5
Furane resin Viscosity-average molecular weight 4000-6000 ????15-25
Resins, epoxy E-44 ????5-10
The oxidized bitumen powder Less than 147 μ m ????8-15
Ethanol Technical pure ????2-8
Acetone Technical pure ????2-8
Ethyl acetate Technical pure ????1-5
Sulfuric acid acetate Technical pure ????2-5
Phosphoric acid second fat Technical pure ????2-5
Table 4 second layer paste formula 4.
Title Specification Weight percentage (%)
TiB 2Powder 3-10μm ????20-40
Petroleum coke powder Less than 147 μ m 147-246 μ m ????10-20 ????5-15
Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????0.8-2
The carbon fiber bar powder Less than 74 μ m ????1-3
Furane resin Viscosity-average molecular weight 4000-6000 ????15-20
Resins, epoxy E-44 ????3-8
The oxidized bitumen powder Less than 147 μ m ????5-10
Ethanol Technical pure ????2-8
Acetone Technical pure ????2-8
Ethyl acetate Technical pure ????1-5
Sulfuric acid acetate Technical pure ????1-3
Phosphoric acid second fat Technical pure ????1-3
The 3rd layer of paste formula of table 5 5.
Title Specification Weight percentage (%)
TiB 2Powder 3-10μm ????50-80
Petroleum coke powder Less than 147 μ m 147-246 μ m ????5-10 ????3-8
Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????0.3-1
The carbon fiber bar powder Less than 74 μ m ????0.5-1
Furane resin Viscosity-average molecular weight 4000-6000 ????5-15
Resins, epoxy E-44 ????1-5
The oxidized bitumen powder Less than 147 μ m ????3-8
Ethanol Technical pure ????2-8
Acetone Technical pure ????2-8
Ethyl acetate Technical pure ????1-5
Sulfuric acid acetate Technical pure ????0.3-1
Phosphoric acid second fat Technical pure ????0.2-1
1. the prescription of coating thickener can multilayer be smeared in actual applications, when keeping good mechanical property, obtains thicker coating, generally as long as the brushing layer 2-3 just can the good cathode material of obtained performance.
2. preparation method's main points are amount and solidified temperature increasing schedules of solidifying agent in every layer of thickener of control.The curing agent content of the lowest layer is the highest, and set time is the fastest, and solidification value is the highest, successively decreases successively then.
3. the streak method multilayer is smeared TiB 2The method of coating prepares the gradient function cathode material, carbon of each layer and TiB 2Content is all different, the lowest layer that contacts with carbon cathode, and carbon content is the highest, successively decreases the TiB of surface layer then successively 2Content is the highest.The composition of coating changes in gradient, causes the performance of cathode material to change in gradient.
Advantage of the present invention and positively effect fully show as:
The present invention reduces TiB 2The deformation of coating in carbonization process; Improved TiB 2The bonding strength of coating and aluminium electrolytic cell cathode carbon liner; Obtain the good coated cathode material of thermal shock resistance; Its surface is moistening fully with aluminium liquid, has prolonged the work-ing life of aluminum electrolyzing cell used titanium boride cathode material and coating.
Be further described below in conjunction with embodiment.
Example 1: smear double-deck gradient function negative electrode.
The end, surface layer paste formula see Table 6,7.
Table 6 bottom paste formula example
Title Specification Weight percentage (%)
TiB 2Powder 3-10μm ????22
Petroleum coke powder Less than 147 μ m 147-246 μ m ????17 ????14
Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????1.2
The carbon fiber bar powder Less than 74 μ m ????1.8
Furane resin Viscosity-average molecular weight 4000-6000 ????14.5
Resins, epoxy E-44 ????7.5
Title Specification Weight percentage (%)
The oxidized bitumen powder Less than 147 μ m ????11
Ethanol Technical pure ????3
Acetone Technical pure ????2.8
Ethyl acetate Technical pure ????2.2
Sulfuric acid acetate Technical pure ????1.8
Phosphoric acid second fat Technical pure ????1.2
Table 7 surface layer paste formula example
Title Specification Weight percentage (%)
TiB 2Powder 3-10μm ????56
Petroleum coke powder Less than 147 μ m 147-246 μ m ????8 ????7
Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????0.5
The carbon fiber bar powder Less than 74 μ m ????1.5
Furane resin Viscosity-average molecular weight 4000-6000 ????7
Resins, epoxy E-44 ????4
The oxidized bitumen powder Less than 147 μ m ????6
Ethanol Technical pure ????3.7
Acetone Technical pure ????3
Title Specification Weight percentage (%)
Ethyl acetate Technical pure ????2
Sulfuric acid acetate Technical pure ????0.75
Phosphoric acid second fat Technical pure ????0.55
By dosage in the table, the good coating thickener of mixed configuration is applied in thickener on the cathode carbon pieces, and according to aforesaid curing, charing temperature increasing schedule, curing, charing coating, the bonding strength of gained coating is greater than the tensile strength (2.7 ± 0.2MPa) of matrix carbon cathode; From 25 ℃, 40 minutes, be rapidly heated to 900 ℃, reduce to 25 ℃ rapidly from 900 ℃ again, capable of circulation more than 8 times; With aluminium liquid complete wetting; Thickness reaches more than the 10mm.
Example 2: smear trilaminar gradient function negative electrode.
The end, surface layer paste formula see Table 8,9,10.
Table 8 bottom paste formula example
Title Specification Weight percentage (%)
TiB 2Powder 3-10μm ????9.5
Petroleum coke powder Less than 147 μ m 147-246 μ m ????21 ????11.5
Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????2
The carbon fiber bar powder Less than 74 μ m ????3.5
Furane resin Viscosity-average molecular weight 4000-6000 ????16.5
Resins, epoxy E-44 ????7
Title Specification Weight percentage (%)
The oxidized bitumen powder Less than 147 μ m ????12
Ethanol Technical pure ????5
Acetone Technical pure ????3.5
Ethyl acetate Technical pure ????3
Sulfuric acid acetate Technical pure ????3.2
Phosphoric acid second fat Technical pure ????2.3
Table 9 second layer paste formula example
Title Specification Weight percentage (%)
TiB 2Powder 3-10μm ????30
Petroleum coke powder Less than 147 μ m 147-246 μ m ????18 ????8.5
Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????1.2
The carbon fiber bar powder Less than 74 μ m ????1.7
Furane resin Viscosity-average molecular weight 4000-6000 ????14.5
Resins, epoxy E-44 ????6
The oxidized bitumen powder Less than 147 μ m ????8
Ethanol Technical pure ????4
Acetone Technical pure ????3.5
Title Specification Weight percentage (%)
Ethyl acetate Technical pure ????2.8
Sulfuric acid acetate Technical pure ????1
Phosphoric acid second fat Technical pure ????1
Table 10 surface layer paste formula example
Title Specification Weight percentage (%)
TiB 2Powder 3-10μm ????62
Petroleum coke powder Less than 147 μ m 147-246 μ m ????6.5 ????4
Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????0.4
The carbon fiber bar powder Less than 74 μ m ????0.5
Furane resin Viscosity-average molecular weight 4000-6000 ????7.5
Resins, epoxy E-44 ????3
The oxidized bitumen powder Less than 147 μ m ????5.5
Ethanol Technical pure ????4
Acetone Technical pure ????3
Ethyl acetate Technical pure ????2.8
Sulfuric acid acetate Technical pure ????0.4
Phosphoric acid second fat Technical pure ????0.3
By dosage in the table, the good coating thickener of mixed configuration is applied in thickener on the cathode carbon pieces, according to aforesaid curing, charing temperature increasing schedule, and curing, charing coating, the bonding strength of gained coating is greater than the tensile strength (2.7 ± 0.2MPa) of matrix carbon cathode; From 25 ℃, in 40 minutes, be rapidly heated to 900 ℃, reduce to 25 ℃ rapidly from 900 ℃ again, capable of circulation more than 10 times; With aluminium liquid complete wetting; Thickness reaches more than the 10mm; Flawless.

Claims (3)

1. the preparation method of titanium boride cathode material with gradient function of aluminium electrolytic bath is that the single prescription with the cathode of aluminium electrolytic bath titanium boride coating changes multiple formulations into, and the disposable squeegee process of individual layer changes multilayer into and smears preparation method, it is characterized in that:
One, smears the preparation method of two layers of thickener
(1) smear first coating with the titanium boride thickener of filling a prescription 1. on cathode of aluminium electrolytic bath, it is 25-60 ℃ that temperature increasing schedule is solidified in control: 10 ℃/h; 60-120 ℃: 5 ℃/h; 120-180 ℃: 9 ℃/h; 180-220 ℃: 6 ℃/h; 220-280 ℃: 8 ℃/h;
(2) smear second coating with the titanium boride thickener of filling a prescription 2. on cathode of aluminium electrolytic bath, it is 25-60 ℃ that temperature increasing schedule is solidified in control: 10 ℃/h; 60-120 ℃: 4 ℃/h; 120-180 ℃: 8 ℃/h; 180-210 ℃: 5 ℃/h;
(3) control charing temperature increasing schedule is 25-300 ℃: 25 ℃/h; 300-600 ℃: 8 ℃/h; 600-900 ℃: 12 ℃/h.
Perhaps:
Two, smear the preparation method of three layers of thickener
(4) smear first coating with the titanium boride thickener of filling a prescription 3. on cathode of aluminium electrolytic bath, it is 25-60 ℃ that temperature increasing schedule is solidified in control: 12 ℃/h; 60-120 ℃: 8 ℃/h; 120-180 ℃: 10 ℃/h; 180-220 ℃: 8 ℃/h; 220-300 ℃: 10 ℃/h.
(5) smear second coating with the titanium boride thickener of filling a prescription 4. on cathode of aluminium electrolytic bath, it is 25-60 ℃ that temperature increasing schedule is solidified in control: 9 ℃/h; 60-120 ℃: 5 ℃/h; 120-180 ℃: 9 ℃/h; 180-220 ℃: 6 ℃/h; 220-250 ℃: 7 ℃/h;
(6) smear the 3rd coating with the titanium boride thickener of filling a prescription 5. on cathode of aluminium electrolytic bath, it is 25-60 ℃ that temperature increasing schedule is solidified in control: 10 ℃/h; 60-120 ℃: 4 ℃/h; 120-180 ℃: 8 ℃/h; 180-210 ℃: 5 ℃/h;
(7) control carbonization temperature increasing schedule is 25-300 ℃: 25 ℃/h; 300-600 ℃: 8 ℃/h; 600-900 ℃: 12 ℃/h.
2. the preparation method of titanium boride cathode material with gradient function of aluminium electrolytic bath according to claim 1, it is characterized in that: the prescription of two layers of smearing method is shown in table 1,2:
Table 1 the first layer paste formula 1. Title Specification Weight percentage (%) TiB 2Powder 3-10μm ????10-30 Petroleum coke powder Less than 147 μ m 147-246 μ m ????15-30 ????5-15 Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????0.5-1 The carbon fiber bar powder Less than 74 μ m ????1-2 Furane resin Viscosity-average molecular weight 4000-6000 ????15-20 Resins, epoxy E-44 ????5-10 The oxidized bitumen powder Less than 147 μ m ????8-15 Ethanol Technical pure ????2-8 Acetone Technical pure ????2-8 Ethyl acetate Technical pure ????1-5 Sulfuric acid acetate Technical pure ????1-3 Phosphoric acid second fat Technical pure ????1-3
Table 2 second layer paste formula 2. Title Specification Weight percentage (%) TiB 2Powder 3-10μm ????40-70 Petroleum coke powder Less than 147 μ m 60 less than 147 μ m ????5-15 ????3-8 Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????0.5-1 The carbon fiber bar powder Less than 74 μ m ????1-2 Furane resin Viscosity-average molecular weight 4000-6000 ????10-15 Resins, epoxy E-44 ????3-8 The oxidized bitumen powder Less than 147 μ m ????5-10 Ethanol Technical pure ????2-8 Acetone Technical pure ????2-8 Ethyl acetate Technical pure ????1-5 Sulfuric acid acetate Technical pure ????0.5-2 Phosphoric acid second fat Technical pure ????0.5-2
The prescription of render float and set method such as table 3,4,5:
3. the preparation method of titanium boride cathode material with gradient function of aluminium electrolytic bath according to claim 1 is characterized in that: the prescription of render float and set method such as table 3,4,5:
Table 3 the first layer paste formula 3. Title Specification Weight percentage (%) TiB 2Powder 3-10μm ????5-15 Petroleum coke powder Less than 147 μ m 147-246 μ m ????20-40 ????10-20 Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????1-3 The carbon fiber bar powder Less than 74 μ m ????2-5 Furane resin Viscosity-average molecular weight 4000-6000 ????15-25 Resins, epoxy E-44 ????5-10 The oxidized bitumen powder Less than 147 μ m ????8-15 Ethanol Technical pure ????2-8 Acetone Technical pure ????2-8 Ethyl acetate Technical pure ????1-5 Sulfuric acid acetate Technical pure ????2-5 Phosphoric acid second fat Technical pure ????2-5
Table 4 second layer paste formula 4. Title Specification Weight percentage (%) TiB 2Powder 3-10μm ????20-40 Petroleum coke powder Less than 147 μ m 147-246 μ m ????10-20 ????5-15 Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????0.8-2 The carbon fiber bar powder Less than 74 μ m ????1-3 Furane resin Viscosity-average molecular weight 4000-6000 ????15-20 Resins, epoxy E-44 ????3-8 The oxidized bitumen powder Less than 147 μ m ????5-10 Ethanol Technical pure ????2-8 Acetone Technical pure ????2-8 Ethyl acetate Technical pure ????1-5 Sulfuric acid acetate Technical pure ????1-3 Phosphoric acid second fat Technical pure ????1-3
The 3rd layer of paste formula of table 5 5. Title Specification Weight percentage (%) TiB 2Powder 3-10μm ????50-80 Petroleum coke powder Less than 147 μ m 147-246 μ m ????5-10 ????3-8 Carbon fiber bar Single diameter 6-7 μ m, length 3-5cm ????0.3-1 The carbon fiber bar powder Less than 74 μ m ????0.5-1 Furane resin Viscosity-average molecular weight 4000-6000 ????5-15 Resins, epoxy E-44 ????1-5 The oxidized bitumen powder Less than 147 μ m ????3-8 Ethanol Technical pure ????2-8 Acetone Technical pure ????2-8 Ethyl acetate Technical pure ????1-5 Sulfuric acid acetate Technical pure ????0.3-1 Phosphoric acid second fat Technical pure ????0.2-1
CN 02107239 2002-03-13 2002-03-13 Preparation method of titanium boride cathode material with gradient function of aluminium electrolytic bath Expired - Fee Related CN1203216C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101844926A (en) * 2010-03-24 2010-09-29 中南大学 Pelleting method of titanium diboride powder

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101844926A (en) * 2010-03-24 2010-09-29 中南大学 Pelleting method of titanium diboride powder
CN101844926B (en) * 2010-03-24 2012-11-07 中南大学 Pelleting method of titanium diboride powder

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