CN106186685A - 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
CN106186685A
CN106186685A CN201610595399.1A CN201610595399A CN106186685A CN 106186685 A CN106186685 A CN 106186685A CN 201610595399 A CN201610595399 A CN 201610595399A CN 106186685 A CN106186685 A CN 106186685A
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purity
oxide
acid
quartz tube
purple
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CN106186685B (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

Abstract

The present invention is a kind of purple quartz tube and preparation method thereof, and it is prepared from the following raw materials in parts by weight: high-purity potassium oxide 0.05 0.08;High-purity sodium oxide 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 less than 30ppm glass sand 99.0 99.5.The present invention can be directly produced prepared purple quartz tube, has good coloring effect, it is not necessary to processes colourless quartz ampoule spray colouration;The present invention uses the mixed acid that hydrochloric acid, Fluohydric acid. and nitric acid are made into simultaneously, when high-temperature baking, decreases the pollution to surrounding and continuous induction melting furnace uses cycle stretch-out one times.

Description

A kind of purple quartz tube and preparation method thereof
Technical field
The present invention relates to a kind of quartz ampoule, particularly a kind of purple quartz tube and preparation method thereof.
Background technology
At present, quartz ampoule, due to its excellent physicochemical property, is widely used in electric light source, quasiconductor, optic communication, army The every field such as work, metallurgy, building materials, chemistry, machinery, electric power, environmental protection, it has Heat stability is good, can bear violent temperature Change, is heated to quartz ampoule about 1100 DEG C, puts in normal-temperature water and also will not burst;Electrical insulation capability is good, is fabulous electricity Insulant, even if the most also having good insulating properties, but the dispensing of existing quartz ampoule is all nitrate dissolves After mixing, high-temperature baking, the nitrogen oxide that during high temperature, nitrate decomposes is very serious to air pollution, and decreases continuous smelting The production cycle of stove.Meanwhile, the quartz ampoule that the production method of quartz ampoule of the prior art is produced is colourless quartz glass Pipe, its production technology controllability is poor, and hydroxy radical content is higher, it is impossible to be satisfied with some special industry demands, and between being typically Having a rest property produces, and production efficiency is relatively low, when needs purple quartz tube, just does coating on colourless quartz ampoule, makes external coating purple Quartz ampoule;Not only complex process, and quality is wayward.
Summary of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, proposes one and produces non-environmental-pollution, can Extend continuous induction melting furnace purple quartz tube using the cycle and preparation method thereof.
The technical problem to be solved in the present invention is achieved through the following technical solutions.The present invention is a kind of violet quartz Pipe, is characterized in, it is prepared from the following raw materials in parts by weight: high-purity potassium oxide 0.05-0.08;High-purity sodium oxide 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 less than 30ppm glass sand 99.0-99.5.
In one purple quartz tube technical scheme of the present invention, further preferred technical scheme feature is:
1, high-purity potassium oxide 0.05;High-purity sodium oxide 0.04;High purity aluminium oxide 0.03;High-purity titanium oxide 0.12;High-purity neodymium oxide 0.08;Impurity content is less than 30ppm glass sand 99.0;
2, high-purity potassium oxide 0.08;High-purity sodium oxide 0.06;High purity aluminium oxide 0.05;High-purity titanium oxide 0.14;High-purity neodymium oxide 0.1;Impurity content is less than 30ppm glass sand 99.5;
3, high-purity potassium oxide 0.07;High-purity sodium oxide 0.05;High purity aluminium oxide 0.04;High-purity titanium oxide 0.13;High-purity neodymium oxide 0.09;Impurity content is less than 30ppm glass sand 99.3.
The technical problem to be solved in the present invention is achieved through the following technical solutions.The present invention is a kind of purple quartz tube Preparation method, be characterized in, comprise the steps: (1) raw material roasting: quartzy former stone is added in quartz ampoule roaster and roasts Burning, quartz ampoule calciner temperature is 900-1000 DEG C, and the rotating speed of quartz ampoule roaster is 15-20 Hz, and load is 50-60Kg/ h;(2) raw material break process: quartzy former stone is pulverized through pulverizer, and through high magnetic that disposal ability is 100-150 Kg/h Machine removes ferrum, and the granularity and the mass percent thereof that obtain quartz sand are as follows:
190-154 micron≤5%;
154-128 micron 10-30%;
128-100 micron 70-90%;
77-100 micron 3-5%;
(3) pickling: above-mentioned quartz sand is mixed in the sourest bubble machine by the weight ratio of 2.4-3:1.5 with mixed acid, stirring Acid bubble 20-24 hour, acid bubble temperature is 30-40 DEG C;The wherein mixed acid hydrochloric acid with mass percent concentration as 31-35%, 42- The Fluohydric acid. of 44% and the nitric acid of 61-67% are raw material, and the weight ratio of hydrochloric acid, Fluohydric acid., nitric acid is 4-5:1.3-1.6:0.2; Ultra-pure water is used to be carried out after pickling is complete;(4) dry: use dehydrator continuous oven drying, dry temperature and be 1000-1050 DEG C, Speed of shaking out is 50-80Kg/h, and rear cooling obtains impurity content less than 30ppm glass sand;(5) element doping: weigh and receive The other high-purity potassium oxide 0.05-0.08 of meter level, high-purity sodium oxide 0.04-0.06, high purity aluminium oxide 0.03-0.05, high pure zirconia Titanium 0.12-0.14 and high-purity neodymium oxide 0.08-0.1, feeds the mixture into after stirring in agitator, adds impurity content Less than 30ppm glass sand 99.0-99.5 mix and blend, speed of agitator is 300-500 r/h, and mixing time is 5-6 h; (6) by the quartz sand pack after stirring, it is subsequently adding continuous induction melting furnace trombone slide at 2200-2300 DEG C, i.e. can get uniform purple Quartz ampoule.
In the preparation method technical scheme of a kind of purple quartz tube of the present invention, further preferred technical scheme feature is:
1, in described step (1), quartz ampoule calciner temperature is 950 DEG C, and the rotating speed of quartz ampoule roaster is 17Hz, and load is 55Kg/h;
2, in described step (3), quartz sand is mixed in the sourest bubble machine by the weight ratio of 2.7:1.5 with mixed acid, stirring acid bubble 22 Hour, acid bubble temperature is 35 DEG C;Wherein the mixed acid hydrochloric acid with mass percent concentration as 31-35%, the Fluohydric acid. of 42-44% and The nitric acid of 61-67% is raw material, and the weight ratio of hydrochloric acid, Fluohydric acid., nitric acid is 4.5:1.4:0.2;18M Ω is used after pickling is complete Ultra-pure water is carried out;
3, drying temperature in described step (4) is 1020 DEG C, and speed of shaking out is 65Kg/h;
4, in described step (5), speed of agitator is 400r/h, and mixing time is 5.5 h;
5, in described step (6), trombone slide temperature is 2250 DEG C.
Compared with prior art, the present invention can be directly produced prepared purple quartz tube, has good coloring effect, it is not necessary to Colourless quartz ampoule spray colouration is processed;The present invention uses the mixed acid that hydrochloric acid, Fluohydric acid. and nitric acid are made into simultaneously, dries at high temperature Time roasting, decrease the pollution to surrounding and continuous induction melting furnace uses cycle stretch-out one times.
Detailed description of the invention
Further describe the concrete technical scheme of the present invention, in order to those skilled in the art is further understood that this Bright, and do not constitute the restriction 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 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 less than 30ppm glass sand 99.0-99.5.
Embodiment 2, in the purple quartz tube described in embodiment 1: high-purity potassium oxide 0.05;High-purity sodium oxide 0.04;High-purity Aluminium oxide 0.03;High-purity titanium oxide 0.12;High-purity neodymium oxide 0.08;Impurity content is less than 30ppm glass sand 99.0.
Embodiment 3, in the purple quartz tube described in embodiment 1 or 2: high-purity potassium oxide 0.08;High-purity sodium oxide 0.06;High Pure alumina 0.05;High-purity titanium oxide 0.14;High-purity neodymium oxide 0.1;Impurity content is less than 30ppm glass sand 99.5.
Embodiment 4, in the purple quartz tube described in any one of embodiment 1-3: high-purity potassium oxide 0.07;High-purity sodium oxide 0.05;High purity aluminium oxide 0.04;High-purity titanium oxide 0.13;High-purity neodymium oxide 0.09;Impurity content is less than 30ppm glass sand 99.3。
Embodiment 5, the preparation method of a kind of purple quartz tube, comprise the steps: (1) raw material roasting: by quartzy former stone Adding quartz ampoule roasting kiln roasting, quartz ampoule calciner temperature is 900-1000 DEG C, and the rotating speed of quartz ampoule roaster is 15-20 Hz, load is 50-60Kg/h;(2) raw material break process: quartzy former stone is pulverized through pulverizer, and through disposal ability High magnetomechanical for 100-150 Kg/h removes ferrum, and the granularity and the mass percent thereof that obtain quartz sand are as follows:
190-154 micron≤5%;
154-128 micron 10-30%;
128-100 micron 70-90%;
77-100 micron 3-5%;
The thinnest rank of quartz sand of raw material granularity compared with normal, it is simple to batch mixing and melted time mix with doped raw material and melt Uniformly;(3) pickling: above-mentioned quartz sand is mixed in the sourest bubble machine by the weight ratio of 2.4-3:1.5 with mixed acid, stirring Acid bubble 20-24 hour, acid bubble temperature is 30-40 DEG C;The wherein mixed acid hydrochloric acid with mass percent concentration as 31-35%, 42- The Fluohydric acid. of 44% and the nitric acid of 61-67% are raw material, and the weight ratio of hydrochloric acid, Fluohydric acid., nitric acid is 4-5:1.3-1.6:0.2; Ultra-pure water is used to be carried out after pickling is complete;(4) dry: use dehydrator continuous oven drying, dry temperature and be 1000-1050 DEG C, Speed of shaking out is 50-80Kg/h, and rear cooling obtains impurity content less than 30ppm glass sand;(5) element doping: weigh and receive The other high-purity potassium oxide 0.05-0.08 of meter level, high-purity sodium oxide 0.04-0.06, high purity aluminium oxide 0.03-0.05, high pure zirconia Titanium 0.12-0.14 and high-purity neodymium oxide 0.08-0.1, feeds the mixture into after stirring in agitator, adds impurity content Less than 30ppm glass sand 99.0-99.5 mix and blend, speed of agitator is 300-500 r/h, and mixing time is 5-6 h; (6) by the quartz sand pack after stirring, it is subsequently adding continuous induction melting furnace trombone slide at 2200-2300 DEG C, i.e. can get uniform purple Quartz ampoule.
Embodiment 6, in the preparation method of the purple quartz tube described in embodiment 5: quartz ampoule roaster in described step (1) Temperature is 950 DEG C, and the rotating speed of quartz ampoule roaster is 17Hz, and load is 55Kg/h.
Embodiment 7, in the preparation method of the purple quartz tube described in embodiment 5 or 6: in described step (3) quartz sand with Mixed acid is mixed in the sourest bubble machine by the weight ratio of 2.7:1.5, and stirring acid bubble 22 hours, it is 35 DEG C that temperature is steeped in acid;Wherein mix Close the nitric acid of the acid hydrochloric acid, the Fluohydric acid. of 42-44% and 61-67% with mass percent concentration as 31-35% as raw material, and hydrochloric acid, Fluohydric acid., the weight ratio of nitric acid are 4.5:1.4:0.2;18M Ω ultra-pure water is used to be carried out after pickling is complete.
Embodiment 8, in the preparation method of the purple quartz tube described in any one of embodiment 5-7: dry in described step (4) Temperature is 1020 DEG C, and speed of shaking out is 65Kg/h.
Embodiment 9, in the preparation method of the purple quartz tube described in any one of embodiment 5-8: stirring in described step (5) Rotating speed is 400r/h, and mixing time is 5.5 h.
Embodiment 10, in the preparation method of the purple quartz tube described in any one of embodiment 5-9: described step is drawn in (6) Pipe temperature is 2250 DEG C.

Claims (10)

1. a purple quartz tube, it is characterised in 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 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 less than 30ppm glass sand 99.0-99.5.
Purple quartz tube the most according to claim 1, it is characterised in that it is prepared from the following raw materials in parts by weight:
High-purity potassium oxide 0.05;High-purity sodium oxide 0.04;
High purity aluminium oxide 0.03;High-purity titanium oxide 0.12;
High-purity neodymium oxide 0.08;
Impurity content is less than 30ppm glass sand 99.
Purple quartz tube the most according to claim 1, it is characterised in that it is prepared from the following raw materials in parts by weight:
High-purity potassium oxide 0.08;High-purity sodium oxide 0.06;
High purity aluminium oxide 0.05;High-purity titanium oxide 0.14;
High-purity neodymium oxide 0.1;
Impurity content is less than 30ppm glass sand 99.5.
Purple quartz tube the most according to claim 1, it is characterised in that it is prepared from the following raw materials in parts by weight:
High-purity potassium oxide 0.07;High-purity sodium oxide 0.05;
High purity aluminium oxide 0.04;High-purity titanium oxide 0.13;
High-purity neodymium oxide 0.09;
Impurity content is less than 30ppm glass sand 99.3.
5. according to the preparation method of purple quartz tube described in any one of claim 1-4, it is characterised in that comprise the steps:
(1) raw material roasting: quartzy former stone is added quartz ampoule roasting kiln roasting, and quartz ampoule calciner temperature is 900-1000 DEG C, the rotating speed of quartz ampoule roaster is 15-20 Hz, and load is 50-60Kg/h;
(2) raw material break process: quartzy former stone is pulverized through pulverizer, and through height that disposal ability is 100-150 Kg/h Magnetomechanical removes ferrum, and the granularity and the mass percent thereof that obtain quartz sand are as follows:
190-154 micron≤5%;
154-128 micron 10-30%;
128-100 micron 70-90%;
77-100 micron 3-5%;
(3) pickling: above-mentioned quartz sand is mixed in the sourest bubble machine by the weight ratio of 2.4-3:1.5 with mixed acid, stirring Acid bubble 20-24 hour, acid bubble temperature is 30-40 DEG C;The wherein mixed acid hydrochloric acid with mass percent concentration as 31-35%, 42- The Fluohydric acid. of 44% and the nitric acid of 61-67% are raw material, and the weight ratio of hydrochloric acid, Fluohydric acid., nitric acid is 4-5:1.3-1.6:0.2; Ultra-pure water is used to be carried out after pickling is complete;
(4) drying: use dehydrator continuous oven drying, dry temperature and be 1000-1050 DEG C, speed of shaking out is 50-80Kg/h, rear cold But impurity content is obtained less than 30ppm glass sand;
(5) element doping: weigh high-purity potassium oxide 0.05-0.08 of Nano grade, high-purity sodium oxide 0.04-0.06, high pure oxygen Change aluminum 0.03-0.05, high-purity titanium oxide 0.12-0.14 and high-purity neodymium oxide 0.08-0.1, feed the mixture into after stirring In agitator, adding impurity content and be less than 30ppm glass sand 99.0-99.5 mix and blend, speed of agitator is 300-500 R/h, mixing time is 5-6 h;
(6) by the quartz sand pack after stirring, it is subsequently adding continuous induction melting furnace trombone slide at 2200-2300 DEG C, i.e. available uniform Purple quartz tube.
6. according to the preparation method of purple quartz tube described in any one of claim 5, it is characterised in that: stone in described step (1) English pipe calciner temperature is 950 DEG C, and the rotating speed of quartz ampoule roaster is 17Hz, and load is 55Kg/h.
7. according to the preparation method of purple quartz tube described in any one of claim 5, it is characterised in that: stone in described step (3) Sand is mixed in the sourest bubble machine by the weight ratio of 2.7:1.5 with mixed acid, and stirring acid bubble 22 hours, it is 35 DEG C that temperature is steeped in acid; Wherein the nitric acid of mixed acid hydrochloric acid, the Fluohydric acid. of 42-44% and 61-67% with mass percent concentration as 31-35% is as raw material, And the weight ratio of hydrochloric acid, Fluohydric acid., nitric acid is 4.5:1.4:0.2;18M Ω ultra-pure water is used to be carried out after pickling is complete.
8. according to the preparation method of purple quartz tube described in any one of claim 5, it is characterised in that: described step (4) is dried Dry temperature is 1020 DEG C, and speed of shaking out is 65Kg/h.
9. according to the preparation method of purple quartz tube described in any one of claim 5, it is characterised in that: described step is stirred in (5) Mixing rotating speed is 400r/h, and mixing time is 5.5 h.
10. according to the preparation method of purple quartz tube described in any one of claim 5, it is characterised in that: described step is drawn in (6) Pipe temperature 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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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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