CN106186685B - A kind of purple quartz tube and preparation method thereof - Google Patents

A kind of purple quartz tube and preparation method thereof Download PDF

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Publication number
CN106186685B
CN106186685B CN201610595399.1A CN201610595399A CN106186685B CN 106186685 B CN106186685 B CN 106186685B CN 201610595399 A CN201610595399 A CN 201610595399A CN 106186685 B CN106186685 B CN 106186685B
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acid
quartz tube
purity
purple
quartz
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CN106186685A (en
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陶明顿
濮阳坤
赵有文
庞海涛
张尧
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FUDONG LIGHTING LLC
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B20/00Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/06Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00Compositions for glass with special properties
    • C03C4/02Compositions for glass with special properties for coloured glass
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2201/00Glass compositions
    • C03C2201/06Doped silica-based glasses
    • C03C2201/30Doped silica-based glasses containing metals
    • C03C2201/34Doped silica-based glasses containing metals containing rare earth metals
    • C03C2201/36Doped silica-based glasses containing metals containing rare earth metals containing rare earth metals and aluminium, e.g. Er-Al co-doped
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2201/00Glass compositions
    • C03C2201/06Doped silica-based glasses
    • C03C2201/30Doped silica-based glasses containing metals
    • C03C2201/40Doped silica-based glasses containing metals containing transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn
    • C03C2201/42Doped silica-based glasses containing metals containing transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn containing titanium
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2201/00Glass compositions
    • C03C2201/06Doped silica-based glasses
    • C03C2201/30Doped silica-based glasses containing metals
    • C03C2201/50Doped silica-based glasses containing metals containing alkali metals
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2203/00Production processes
    • C03C2203/10Melting processes

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Compositions (AREA)

Abstract

The present invention is a kind of purple quartz tube and preparation method thereof, it is prepared from the following raw materials in parts by weight: high-purity potassium oxide 0.05-0.08;High-purity sodium oxide molybdena 0.04-0.06;High purity aluminium oxide 0.03-0.05;High-purity titanium oxide 0.12-0.14;High-purity neodymium oxide 0.08-0.1;Impurity content is lower than 30ppm glass sand 99.0-99.5.The present invention can directly produce obtained purple quartz tube, have good coloring effect, without handling colourless quartz ampoule spray colouration;The mixed acid that the present invention is made into using hydrochloric acid, hydrofluoric acid and nitric acid simultaneously reduces the pollution to ambient enviroment and continuous induction melting furnace service life extends one times in high-temperature baking.

Description

A kind of purple quartz tube and preparation method thereof
Technical field
The present invention relates to a kind of quartz ampoule, especially a kind of purple quartz tube and preparation method thereof.
Background technique
Currently, quartz ampoule is widely used in electric light source, semiconductor, optic communication, army due to its excellent physicochemical property The every field such as work, metallurgy, building materials, chemistry, machinery, electric power, environmental protection, it is good with thermal stability, violent temperature can be born Variation, is heated to 1100 DEG C or so for quartz ampoule, being put into normal-temperature water will not burst;Electrical insulation capability is good, is fabulous electricity Insulating materials has good insulation performance at high temperature, but the ingredient of existing quartz ampoule is all nitrate dissolution After mixing, high-temperature baking, the nitrogen oxide that nitrate decomposes when high temperature is very serious to air pollution, and reduces continuous smelting The production cycle of furnace.Meanwhile the production method quartz ampoule produced of quartz ampoule in the prior art is colourless quartz glass Pipe, production technology controllability is poor, and hydroxy radical content is higher, cannot be satisfied with some special industry demands, and between being generally The production of having a rest property, production efficiency is lower, when needing purple quartz tube, just does coating on colourless quartz ampoule, external coating purple is made Quartz ampoule;Not only complex process, and quality is not easy to control.
Summary of the invention
It, can the technical problem to be solved by the present invention is in view of the deficiencies of the prior art, propose a kind of production non-environmental-pollution Extend the purple quartz tube and preparation method thereof of continuous induction melting furnace service life.
The technical problem to be solved by the present invention is to what is be achieved through the following technical solutions.The present invention is a kind of violet quartz Pipe, its main feature is that, it is prepared from the following raw materials in parts by weight: high-purity potassium oxide 0.05-0.08;High-purity sodium oxide molybdena 0.04- 0.06;High purity aluminium oxide 0.03-0.05;High-purity titanium oxide 0.12-0.14;High-purity neodymium oxide 0.08-0.1;Impurity content is lower than 30ppm glass sand 99.0-99.5.
In a kind of purple quartz tube technical solution of the present invention, further preferred technical solution is characterized in:
1, high-purity potassium oxide 0.05;High-purity sodium oxide molybdena 0.04;High purity aluminium oxide 0.03;High-purity titanium oxide 0.12;High pure oxygen Change neodymium 0.08;Impurity content is lower than 30ppm glass sand 99.0;
2, high-purity potassium oxide 0.08;High-purity sodium oxide molybdena 0.06;High purity aluminium oxide 0.05;High-purity titanium oxide 0.14;High pure oxygen Change neodymium 0.1;Impurity content is lower than 30ppm glass sand 99.5;
3, high-purity potassium oxide 0.07;High-purity sodium oxide molybdena 0.05;High purity aluminium oxide 0.04;High-purity titanium oxide 0.13;High pure oxygen Change neodymium 0.09;Impurity content is lower than 30ppm glass sand 99.3.
The technical problem to be solved by the present invention is to what is be achieved through the following technical solutions.The present invention is a kind of purple quartz tube Preparation method, its main feature is that, include the following steps: that (1) raw material roasts: the former stone of quartz being added in quartz ampoule roaster and is roasted It burns, quartz ampoule calciner temperature is 900-1000 DEG C, and the revolving speed of quartz ampoule roaster is 15-20Hz, load 50-60Kg/ h;(2) raw material break process: quartzy former stone is crushed by pulverizer, and the high magnetic for being 100-150Kg/h by processing capacity Machine removes iron, and granularity and its mass percent for obtaining quartz sand are as follows:
(3) pickling: above-mentioned quartz sand and mixed acid are mixed into the sour bubble machine of dynamic by the weight ratio of 2.4-3:1.5, Stirring acid bubble 20-24 hours, acid bubble temperature was 30-40 DEG C;Wherein mixed acid is the salt of 31-35% with mass percent concentration The nitric acid of acid, the hydrofluoric acid of 42-44% and 61-67% is raw material, and the weight ratio of hydrochloric acid, hydrofluoric acid, nitric acid is 4-5:1.3- 1.6:0.2;It is cleaned after pickling is complete using ultrapure water;(4) it dries: using dryer continuous drying, drying temperature 1000- 1050 DEG C, speed of shaking out is 50-80Kg/h, and the rear cooling impurity content that obtains is lower than 30ppm glass sand;(5) element doping: Weigh high-purity potassium oxide 0.05-0.08, the high-purity sodium oxide molybdena 0.04-0.06, high purity aluminium oxide 0.03-0.05, height of Nano grade Pure zirconia titanium 0.12-0.14 and high-purity neodymium oxide 0.08-0.1, feeds the mixture into blender after mixing evenly, adds miscellaneous Matter content is mixed lower than 30ppm glass sand 99.0-99.5, speed of agitator 300-500r/h, mixing time 5- 6h;(6) quartz sand after stirring is packed, continuous induction melting furnace trombone slide at 2200-2300 DEG C is then added, uniform purple can be obtained Color quartz ampoule.
In a kind of preparation method technical solution of purple quartz tube of the present invention, further preferred technical solution is characterized in:
1, quartz ampoule calciner temperature is 950 DEG C in the step (1), and the revolving speed of quartz ampoule roaster is Hz, load For 55Kg/h;
2, quartz sand and mixed acid are mixed into the sour bubble machine of dynamic by the weight ratio of 2.7:1.5 in the step (3), stirring acid Bubble 22 hours, acid bubble temperature is 35 DEG C;Wherein mixed acid with mass percent concentration be the hydrochloric acid of 31-35%, the hydrogen of 42-44% The nitric acid of fluoric acid and 61-67% are raw material, and the weight ratio of hydrochloric acid, hydrofluoric acid, nitric acid is 4.5:1.4:0.2;Make after pickling is complete It is cleaned with 18M Ω ultrapure water;
3, drying temperature is 1020 DEG C in the step (4), and speed of shaking out is 65Kg/h;
4, speed of agitator is 400r/h, mixing time 5.5h in the step (5);
5, trombone slide temperature is 2250 DEG C in the step (6).
Compared with prior art, the present invention can directly produce obtained purple quartz tube, have good coloring effect, be not necessarily to Colourless quartz ampoule spray colouration is handled;The mixed acid that the present invention is made into using hydrochloric acid, hydrofluoric acid and nitric acid simultaneously is dried in high temperature When roasting, reduce the pollution to ambient enviroment and continuous induction melting furnace service life extends one times.
Specific embodiment
The specific technical solution of the present invention is further described, in order to which those skilled in the art is further understood that this hair It is bright, without constituting the limitation to its right.
Embodiment 1, a kind of purple quartz tube, it is prepared from the following raw materials in parts by weight: high-purity potassium oxide 0.05- 0.08;High-purity sodium oxide molybdena 0.04-0.06;High purity aluminium oxide 0.03-0.05;High-purity titanium oxide 0.12-0.14;High-purity neodymium oxide 0.08-0.1;Impurity content is lower than 30ppm glass sand 99.0-99.5.
Embodiment 2, in purple quartz tube described in embodiment 1: high-purity potassium oxide 0.05;High-purity sodium oxide molybdena 0.04;It is high-purity Aluminium oxide 0.03;High-purity titanium oxide 0.12;High-purity neodymium oxide 0.08;Impurity content is lower than 30ppm glass sand 99.0.
Embodiment 3, in purple quartz tube described in embodiment 1 or 2: high-purity potassium oxide 0.08;High-purity sodium oxide molybdena 0.06;It is high Pure alumina 0.05;High-purity titanium oxide 0.14;High-purity neodymium oxide 0.1;Impurity content is lower than 30ppm glass sand 99.5.
Embodiment 4, in the described in any item purple quartz tubes of embodiment 1-3: high-purity potassium oxide 0.07;High-purity sodium oxide molybdena 0.05;High purity aluminium oxide 0.04;High-purity titanium oxide 0.13;High-purity neodymium oxide 0.09;Impurity content is lower than 30ppm glass sand 99.3。
Embodiment 5, a kind of preparation method of purple quartz tube include the following steps: that (1) raw material roasts: by quartzy former stone Quartz ampoule is added and roasts kiln roasting, quartz ampoule calciner temperature is 900-1000 DEG C, and the revolving speed of quartz ampoule roaster is 15- 20Hz, load 50-60Kg/h;(2) raw material break process: quartzy former stone is crushed by pulverizer, and by processing energy The high magnetomechanical that power is 100-150Kg/h removes iron, and granularity and its mass percent for obtaining quartz sand are as follows:
The partially thin rank of the more normal quartz sand of raw material granularity, convenient for mixing and melt when mixed with doped raw material and Melt uniform;(3) pickling: above-mentioned quartz sand and mixed acid are mixed into the sour bubble machine of dynamic by the weight ratio of 2.4-3:1.5, Stirring acid bubble 20-24 hours, acid bubble temperature was 30-40 DEG C;Wherein mixed acid is the salt of 31-35% with mass percent concentration The nitric acid of acid, the hydrofluoric acid of 42-44% and 61-67% is raw material, and the weight ratio of hydrochloric acid, hydrofluoric acid, nitric acid is 4-5:1.3- 1.6:0.2;It is cleaned after pickling is complete using ultrapure water;(4) it dries: using dryer continuous drying, drying temperature 1000- 1050 DEG C, speed of shaking out is 50-80Kg/h, and the rear cooling impurity content that obtains is lower than 30ppm glass sand;(5) element doping: Weigh high-purity potassium oxide 0.05-0.08, the high-purity sodium oxide molybdena 0.04-0.06, high purity aluminium oxide 0.03-0.05, height of Nano grade Pure zirconia titanium 0.12-0.14 and high-purity neodymium oxide 0.08-0.1, feeds the mixture into blender after mixing evenly, adds miscellaneous Matter content is mixed lower than 30ppm glass sand 99.0-99.5, speed of agitator 300-500r/h, mixing time 5- 6h;(6) quartz sand after stirring is packed, continuous induction melting furnace trombone slide at 2200-2300 DEG C is then added, uniform purple can be obtained Color quartz ampoule.
Embodiment 6, in the preparation method of purple quartz tube described in embodiment 5: quartz ampoule roaster in the step (1) Temperature is 950 DEG C, and the revolving speed of quartz ampoule roaster is Hz, load 55Kg/h.
Embodiment 7, in the preparation method of purple quartz tube described in embodiment 5 or 6: in the step (3) quartz sand with Mixed acid is mixed into the sour bubble machine of dynamic by the weight ratio of 2.7:1.5, stirs acid bubble 22 hours, and acid bubble temperature is 35 DEG C;Wherein mix Close acid using mass percent concentration for the hydrochloric acid of 31-35%, the hydrofluoric acid of 42-44% and 61-67% nitric acid as raw material, and salt Acid, hydrofluoric acid, nitric acid weight ratio be 4.5:1.4:0.2;It is cleaned after pickling is complete using 18M Ω ultrapure water.
Embodiment 8, in the preparation method of the described in any item purple quartz tubes of embodiment 5-7: drying in the step (4) Temperature is 1020 DEG C, and speed of shaking out is 65Kg/h.
Embodiment 9, in the preparation method of the described in any item purple quartz tubes of embodiment 5-8: stirring in the step (5) Revolving speed is 400r/h, mixing time 5.5h.
Embodiment 10, in the preparation method of the described in any item purple quartz tubes of embodiment 5-9: being drawn in the step (6) Tube temperature degree is 2250 DEG C.

Claims (10)

1. a kind of purple quartz tube, which is characterized in that it is prepared from the following raw materials in parts by weight:
2. purple quartz tube according to claim 1, which is characterized in that it is prepared from the following raw materials in parts by weight:
3. purple quartz tube according to claim 1, which is characterized in that it is prepared from the following raw materials in parts by weight:
4. purple quartz tube according to claim 1, which is characterized in that it is prepared from the following raw materials in parts by weight:
5. the preparation method of purple quartz tube according to claim 1, which comprises the steps of:
(1) raw material roasts: quartz ampoule is added in quartzy former stone and roasts kiln roasting, quartz ampoule calciner temperature is 900-1000 DEG C, the revolving speed of quartz ampoule roaster is 15-20Hz, load 50-60Kg/h;
(2) raw material break process: quartzy former stone is crushed by pulverizer, and the height for being 100-150Kg/h by processing capacity Magnetomechanical removes iron, and granularity and its mass percent for obtaining quartz sand are as follows:
(3) pickling: above-mentioned quartz sand and mixed acid are mixed into the sour bubble machine of dynamic by the weight ratio of 2.4-3:1.5, stirring Acid bubble 20-24 hours, acid bubble temperature is 30-40 DEG C;Wherein hydrochloric acid, 42- of the mixed acid with mass percent concentration for 31-35% 44% hydrofluoric acid and the nitric acid of 61-67% are raw material, and the weight ratio of hydrochloric acid, hydrofluoric acid, nitric acid is 4-5:1.3-1.6: 0.2;It is cleaned after pickling is complete using ultrapure water;
(4) it dries: using dryer continuous drying, drying temperature is 1000-1050 DEG C, and speed of shaking out is 50-80Kg/h, rear cold But impurity content is obtained lower than 30ppm glass sand;
(5) high-purity potassium oxide 0.05-0.08, the high-purity sodium oxide molybdena 0.04-0.06, high pure oxygen of Nano grade element doping: are weighed Change aluminium 0.03-0.05, high-purity titanium oxide 0.12-0.14 and high-purity neodymium oxide 0.08-0.1, feeds the mixture into after mixing evenly In blender, adds impurity content and be mixed lower than 30ppm glass sand 99.0-99.5, speed of agitator 300- 500r/h, mixing time 5-6h;
(6) quartz sand after stirring is packed, continuous induction melting furnace trombone slide at 2200-2300 DEG C is then added, can be obtained uniform Purple quartz tube.
6. the preparation method of purple quartz tube according to claim 5, it is characterised in that: quartz ampoule roasts in the step (1) Burning furnace temperature is 950 DEG C, and the revolving speed of quartz ampoule roaster is 17Hz, load 55Kg/h.
7. the preparation method of purple quartz tube according to claim 5, it is characterised in that: in the step (3) quartz sand with Mixed acid is mixed into the sour bubble machine of dynamic by the weight ratio of 2.7:1.5, stirs acid bubble 22 hours, and acid bubble temperature is 35 DEG C;Wherein mix Close acid using mass percent concentration for the hydrochloric acid of 31-35%, the hydrofluoric acid of 42-44% and 61-67% nitric acid as raw material, and salt Acid, hydrofluoric acid, nitric acid weight ratio be 4.5:1.4:0.2;It is cleaned after pickling is complete using 18M Ω ultrapure water.
8. the preparation method of purple quartz tube according to claim 5, it is characterised in that: drying temperature in the step (4) It is 1020 DEG C, speed of shaking out is 65Kg/h.
9. the preparation method of purple quartz tube according to claim 5, it is characterised in that: speed of agitator in the step (5) For 400r/h, mixing time 5.5h.
10. the preparation method of purple quartz tube according to claim 5, it is characterised in that: trombone slide temperature in the step (6) It is 2250 DEG C.
CN201610595399.1A 2016-07-27 2016-07-27 A kind of purple quartz tube and preparation method thereof Active CN106186685B (en)

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CN112723739A (en) * 2020-12-18 2021-04-30 新沂海福尔通用仪表有限公司 Quartz pull tube and production process thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101805116A (en) * 2010-04-08 2010-08-18 李玉生 Process for producing superfine high-purity quartz glass pipe for high-temperature sensor
CN103771709A (en) * 2014-01-24 2014-05-07 南通惠通纺织器材有限公司 Low-hydroxyl yellow light-filtering quartz tube and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101805116A (en) * 2010-04-08 2010-08-18 李玉生 Process for producing superfine high-purity quartz glass pipe for high-temperature sensor
CN103771709A (en) * 2014-01-24 2014-05-07 南通惠通纺织器材有限公司 Low-hydroxyl yellow light-filtering quartz tube and preparation method thereof

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