CN100424040C - Process of preparing chromium doping tin sphene type coloring material - Google Patents
Process of preparing chromium doping tin sphene type coloring material Download PDFInfo
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- CN100424040C CN100424040C CNB2007100071647A CN200710007164A CN100424040C CN 100424040 C CN100424040 C CN 100424040C CN B2007100071647 A CNB2007100071647 A CN B2007100071647A CN 200710007164 A CN200710007164 A CN 200710007164A CN 100424040 C CN100424040 C CN 100424040C
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- spray gun
- chromium
- tin
- powder
- continuous oven
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Abstract
This invention discloses a preparation method for chrome doped tin nitre color materials, which adds silicon tetrathoxide, CaCl and SnCl in terms of equal mol ratio and small amount of CrNO3 into ethanol and water in the volume ratio of 30:70 and mixes them uniformly, pulverizes the mixed solution to drops by a jet to dry and thermal-analyze it in a furnace of continuous high temperature to be filtered by a 16-25mum glassiness filter by vacuumizing at the end of the furnace then to calcine the filtered powder in a calcine furnace for 3h to cooled to room temperature and ball-mill it to 8-12mum to get the ceramic color material.
Description
Technical field
The present invention relates to a kind of preparation technology who is used for the chromium doped tin aspidelite type ceramic pigment of ceramic glaze and blank.
Background technology
Be accompanied by the development of ceramic industry and building decorating industry and the raising of people's esthetic sentiment, the chromium doped tin aspidelite type pink ceramic pigment demand that is used for ceramic glaze and blank sharply increases.At present, the industrial chromium doped tin aspidelite type pink ceramic pigment of producing all is to adopt traditional production technique: with calcium oxide (CaO), silicon-dioxide (SiO
2), tindioxide (SnO
2) carry out proportioning by equimolar amount, add small amounts zirconium (Cr on this basis
2O
3) and with above-mentioned raw materials evenly grinding in agate mortar, then ground blended stock is put into High Temperature Furnaces Heating Apparatus and calcine, will calcine good colorant at last by being ground to the granularity that needs, i.e. formation has zinntitanite (CaSnS
iO
5) colorant of structure.This traditional technology has following shortcoming: be to need high calcining temperature on producing on the one hand, each oxide compound at high temperature reacts incomplete on the other hand; Later in order to reduce calcining temperature and to make each oxide compound sufficient reacting, used the muriate of alkali metal containing and alkaline-earth metal in the production, fluorochemical, nitrate, borate and carbonate etc., and the gas that these salt things are produced after at high temperature decomposing can have a strong impact on environment.Other synthetic route, as sol-gel method, coprecipitation method and impregnation technology etc. all exists the cost height to some extent, disadvantage such as the low or technology of product turnover ratio is tediously long.
Summary of the invention
The object of the present invention is to provide that a kind of cost is low, technological process is simple, the technology of preparation chromium doped tin aspidelite type colorant that easily produce, promptly adopts the spraying thermolysis and in conjunction with high-temperature calcination prepared chromium doped tin aspidelite type ceramic pigment.
The present invention's tetraethoxide silicon (＞98%), calcium chloride (CaCl
22H
2O) (＞99%), tin chloride (SnCl
45H
2O) (＞98%) three kinds of raw materials such as press at mol ratio and a small amount of chromium nitrate (Cr (NO
3)
39H
2O) (＞99%) together to join volume ratio be in 30: 70 the ethanol and the aqueous solution and mix; By spray gun above-mentioned mixed solution is atomized into drop and in the continuous high temperature stove, carries out drying and thermolysis, filter by the powder that obtained after vacuumizing dry and thermolysis glassiness strainer simultaneously by 16～25 microns at the afterbody of continuous oven, after powder after then will filtering is put into the high-temperature calcination stove and is calcined 3 hours, cool to room temperature, and powder ball milling to 8～12 micron are promptly made the ceramic pigment with zinntitanite type structure.
In preparation process, because tetraethoxide silicon is water insoluble, so need earlier with second alcohol and water wiring solution-forming; In addition, too high and influence safety and product is collected in order to prevent gas that spraying drying and thermolysis produce at the stove internal gas pressure, also need vacuumize and place a glassiness strainer at the afterbody of continuous calcining stove with 16～25 microns.
Concrete steps are as follows:
(1) be raw material with tetraethoxide silicon, calcium chloride, tin chloride and chromium nitrate, tetraethoxide silicon, calcium chloride, tin chloride are calculated the quality of used each raw material respectively by equimolar amount, allocating it into volume ratio is in 30: 70 the solution of second alcohol and water; The amount of chromium nitrate is according to the color adjustment of needed ceramic pigment, and mol ratio is Cr (NO
3)
39H
2O: CaCl
22H
2O=0.02～0.044: 1;
(2) mixing solutions for preparing is poured in the spray gun liquid-inlet pipe, and stirred, at the inlet mouth access 0.3～0.8kg/cm of spray gun
2Pressurized air;
(3) leading portion at continuous oven is warmed up to 250 ℃, and back segment is warmed up to 600 ℃, keeps the constant of two sections temperature of continuous oven;
(4) open spray gun and mixing solutions is sprayed carry out drying in the stove and atomizing is decomposed, filter by the powder that obtained after vacuumizing drying and thermolysis glassiness strainer at the afterbody of continuous oven simultaneously by 16～25 microns;
(5) powder after will filtering is put into Platinum crucible, puts into High Temperature Furnaces Heating Apparatus (10 ℃/minute of heat-up rates) 1200 ℃ of following high-temperature calcinations 3 hours, and then ball milling to 8～12 micron promptly obtain ceramic pigment with chromium doped tin aspidelite type structure.
Cost of the present invention is low, process control procedure is simple, easily produce, the ceramic pigment powder diameter that makes with chromium doped tin aspidelite type structure evenly, controllable component, purity height.
Embodiment
Embodiment 1:
With tetraethoxide silicon (＞98%), calcium chloride (CaCl
22H
2O) (＞99%), tin chloride (SnCl
45H
2O) (＞98%) and chromium nitrate (Cr (NO
3)
39H
2O) (＞99%) is raw material, makes the pink ceramic pigment with chromium doped tin aspidelite type structure in conjunction with high-temperature calcination technology with the spraying thermolysis.
(1) takes by weighing quality and be respectively 212 grams, 147 grams, the tetraethoxide silicon (＞98%) of 350 grams, calcium chloride (CaCl
22H
2O) (＞99%), tin chloride (SnCl
45H
2O) (＞98%) three kinds of raw materials put it into and have volume and be respectively in the water of 30 milliliters ethanol and 70 milliliters and be made into mixing solutions, and the chromium nitrates that add 12 grams stir together;
(2) mixing solutions for preparing is poured in the spray gun liquid-inlet pipe, and stirred, at the inlet mouth access 0.3～0.8kg/cm of spray gun
2Pressurized air;
(3) leading portion at continuous oven is warmed up to 250 ℃, and back segment is warmed up to 600 ℃, keeps the constant of two sections temperature of continuous oven;
(4) open spray gun and mixing solutions is sprayed carry out drying in the stove and atomizing is decomposed, filter by the powder that obtained after vacuumizing drying and thermolysis glassiness strainer at the afterbody of continuous oven simultaneously by 16～25 microns;
(5) powder after will filtering is put into Platinum crucible, puts into High Temperature Furnaces Heating Apparatus (10 ℃/minute of heat-up rates) 1200 ℃ of following high-temperature calcinations 3 hours, and then ball milling to 8～12 micron promptly obtain ceramic pigment with chromium doped tin aspidelite type structure.
Embodiment 2:
With tetraethoxide silicon (＞98%), calcium chloride (CaCl
22H
2O) (＞99%), tin chloride (SnCl
45H
2O) (＞98%) and chromium nitrate (Cr (NO
3)
39H
2O) (＞99%) is raw material, makes the ceramic pigment with chromium doped tin aspidelite type structure in conjunction with high-temperature calcination technology with the spraying thermolysis.
(1) takes by weighing quality and be respectively 21.2 grams, 14.7 grams, the tetraethoxide silicon (＞98%) of 35 grams, calcium chloride (CaCl
22H
2O) (＞99%), tin chloride (SnCl
45H
2O) (＞98%) three kinds of raw materials put it into and have volume and be respectively in the water of 3 milliliters ethanol and 7 milliliters and be made into mixing solutions, and the chromium nitrates that add 1.5 grams stir together;
(2) mixing solutions for preparing is poured in the spray gun liquid-inlet pipe, and stirred, at the inlet mouth access 0.3～0.8kg/cm of spray gun
2Pressurized air;
(3) leading portion at continuous oven is warmed up to 250 ℃, and back segment is warmed up to 600 ℃, keeps the constant of two sections temperature of continuous oven;
(4) open spray gun and mixing solutions is sprayed carry out drying in the stove and atomizing is decomposed, filter by the powder that obtained after vacuumizing drying and thermolysis glassiness strainer at the afterbody of continuous oven simultaneously by 16～25 microns;
(5) powder after will filtering is put into Platinum crucible, puts into High Temperature Furnaces Heating Apparatus (10 ℃/minute of heat-up rates) 1200 ℃ of following high-temperature calcinations 3 hours, and then ball milling to 8～12 micron promptly obtain ceramic pigment with chromium doped tin aspidelite type structure.
Claims (1)
1. the preparation technology of a chromium doped tin aspidelite type colorant is characterized in that the steps include:
(1) be raw material with tetraethoxide silicon, calcium chloride, tin chloride and chromium nitrate, tetraethoxide silicon, calcium chloride, tin chloride are calculated the quality of used each raw material respectively by equimolar amount, allocating it into volume ratio is in 30: 70 the solution of second alcohol and water; The amount of chromium nitrate is according to the color adjustment of needed ceramic pigment, and mol ratio is for being Cr (NO
3)
39H
2O: CaCl
22H
2O=0.02～0.044: 1;
(2) mixing solutions for preparing is poured in the spray gun liquid-inlet pipe, and stirred, at the inlet mouth access 0.3～0.8kg/cm of spray gun
2Pressurized air;
(3) leading portion at continuous oven is warmed up to 250 ℃, and back segment is warmed up to 600 ℃, keeps the constant of two sections temperature of continuous oven;
(4) open spray gun and mixing solutions is sprayed carry out drying in the stove and atomizing is decomposed, filter by the powder that obtained after vacuumizing drying and thermolysis glassiness strainer at the afterbody of continuous oven simultaneously by 16～25 microns;
(5) powder after will filtering is put into Platinum crucible, puts into High Temperature Furnaces Heating Apparatus 1200 ℃ of following high-temperature calcinations 3 hours, and then ball milling to 8～12 micron promptly obtain ceramic pigment with chromium doped tin aspidelite type structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100071647A CN100424040C (en) | 2007-02-05 | 2007-02-05 | Process of preparing chromium doping tin sphene type coloring material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100071647A CN100424040C (en) | 2007-02-05 | 2007-02-05 | Process of preparing chromium doping tin sphene type coloring material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101033138A CN101033138A (en) | 2007-09-12 |
| CN100424040C true CN100424040C (en) | 2008-10-08 |
Family
ID=38729907
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100071647A Expired - Fee Related CN100424040C (en) | 2007-02-05 | 2007-02-05 | Process of preparing chromium doping tin sphene type coloring material |
Country Status (1)
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|---|---|
| CN (1) | CN100424040C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609897B (en) * | 2014-12-05 | 2016-06-22 | 美轲（广州）化学股份有限公司 | Gold glaze for building and preparation and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1408676A (en) * | 2001-09-19 | 2003-04-09 | 云南锡业集团有限责任公司研究设计院 | Process for producing tin base ceramic pigment |
-
2007
- 2007-02-05 CN CNB2007100071647A patent/CN100424040C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1408676A (en) * | 2001-09-19 | 2003-04-09 | 云南锡业集团有限责任公司研究设计院 | Process for producing tin base ceramic pigment |
Non-Patent Citations (6)
| Title |
|---|
| 化学共沉淀法制备铬锡红色料的研究. 俞康泰等.中国陶瓷，第34卷第6期. 1998 |
| 化学共沉淀法制备铬锡红色料的研究. 俞康泰等.中国陶瓷，第34卷第6期. 1998 * |
| 着色剂对Cr_Sn红陶瓷颜料的影响. 杨萍等.陶瓷研究，第12卷第3期. 1997 |
| 着色剂对Cr_Sn红陶瓷颜料的影响. 杨萍等.陶瓷研究，第12卷第3期. 1997 * |
| 锡基含铬陶瓷颜料呈色性能的研究. 李贵佳.陶瓷研究，第13卷第3期. 1998 |
| 锡基含铬陶瓷颜料呈色性能的研究. 李贵佳.陶瓷研究，第13卷第3期. 1998 * |
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| Publication number | Publication date |
|---|---|
| CN101033138A (en) | 2007-09-12 |
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Jiangmen Dowstone Standard Glaze Co., Ltd. Assignor: Guilin University of Technology Contract fulfillment period: 2008.10.10 to 2014.10.10 contract change Contract record no.: 2009440001273 Denomination of invention: Process of preparing chromium doping tin sphene type coloring material Granted publication date: 20081008 License type: Exclusive license Record date: 2009.8.24 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.10.10 TO 2014.10.10; CHANGE OF CONTRACT Name of requester: JIANGMEN CITY DAOSHI STANDAR GLAZE-MAKING CO., LTD Effective date: 20090824 |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20081008 |