CN101805116A - Process for producing superfine high-purity quartz glass pipe for high-temperature sensor - Google Patents
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Abstract
The invention relates to a process for producing a superfine high-purity quartz glass pipe for a high-temperature sensor, which is characterized by comprising the following steps of: finely selecting quartz blocks as raw materials, wherein the particle size of the quartz blocks is 20-30 mm, and the content of SiO2 is above 99%; sequentially carrying out soaking in hydrochloric acid, roasting, water quenching, mechanical pulverization, iron removal, soaking in mixed acid, high-temperature stirring and washing and high-temperature chloridization on the raw materials to obtain high-purity quartz sand; then throwing the high-purity quartz sand in a quartz furnace for smelting, pulling into a quartz glass pipe, and then scouring, cutting, trimming, ultrasonic cleaning and dehydroxylating so that a finished product is obtained. The quartz glass pipe produced and prepared by the process has the superfine and ultrathin features, has the characteristics of high-temperature resistance, molten steel and glass liquid-washing resistance, corrosive resistance, high heat transfer speed, good soaking performance, large strength, long service life, no bursting under shock heating and cooling condition, strong process operability, scale production and the like, and completely accords with the requirements of various performance indexes of the quartz glass pipe used as an outer protective pipe of the high-temperature sensor.
Description
Technical field
The present invention relates to the production technique of a kind of production technique of quartz glass tube, particularly a kind of superfine high-purity quartz glass pipe for high-temperature sensor.
Background technology
In the prior art, the overcoat pillar of pyrostat is the ceramic coat pillar made from stupalith.The defective of traditional ceramic coat pillar is: its heat transfer rate is slower, the soaking poor-performing, and explosion easily under shock heating quenching conditions, anti-molten steel washes away with glass metal, corrosion resistance is relative relatively poor; Therefore, traditional ceramic coat pillar can not satisfy the requirements at the higher level that have pyrostat now.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, provide a kind of technology reasonable, workable, effectively improve the production technique of the superfine high-purity quartz glass pipe for high-temperature sensor of final product quality.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of production technique of superfine high-purity quartz glass pipe for high-temperature sensor, is characterized in, its step is as follows: (1) optimum break is 20-30mm, SiO
2Content is that the quartz wedge more than 99% is a raw material; With raw material drop in the hydrochloric acid that mass percent concentration is 10-30% soak 20-40 hour after, with pure water wash-out hydrochloric acid, until the electric conductivity of wash-out water less than 60us/cm; Get the quartzy material of pickling;
(2) the quartzy material of pickling is dropped in the stoving oven, at 850 ℃ of-900 ℃ of following roasting 3-5 hours, roasting was carried out shrend with pure water after finishing immediately, carries out mechanical disintegration again, sieve 40-140 order silica powder; With high magnetic machine silica powder being carried out deironing then handles;
(3) be to soak 4-6 days in the mixing acid formed of the hydrofluoric acid of the nitric acid of hydrochloric acid, 10-30% of 10-30% and 5-15% by mass percent concentration with the silica powder input after the deironing, the weight ratio of hydrochloric acid, nitric acid, hydrofluoric acid is 1-2: 1-2: 1-2; Soaking the back will soak slurry to be concentrated into concentration be 30-45% under 40-45 ℃; Must soak slurry;
(4) will soak slurry drops in the ultrasonoscope, adding the mixed solution of being made up of kerosene, oleic acid and ethanol again carries out high temperature and mixes and wash under 300-500 ℃ of condition, the weight of mixed solution is for soaking the 15-30% of slurry weight, mix when washing and regulate the pH value to 7.3-7.5 with ammoniacal liquor, kerosene, oleic acid, alcoholic acid weight ratio are 1-2: 1-2: 1-2 in the mixed solution; Must mix the pulp washing material;
(5) will mix the pulp washing material and drop in the chlorination reaction still, and carry out high-temp chlorination and handle mixing the pulp washing material under 500-1400 ℃ of condition, be that the hydrochloric acid of 10-30% carried out high-temperature chlorination 0.5-2.0 hour by chlorine, tetrachloromethane and mass percent concentration during processing; Dry after the reaction, deironing handles, the magneticstrength of high magnetic machine is 1800-2200KA/m during deironing; Get the glass sand of total impurities content less than 30ppm;
(6) after glass sand drops into and carries out melting in the quartz continuous melting furnace, be drawn into the quartz glass tube that diameter is 1.3-1.5; Get quartz glass tube then, using by mass percent concentration is that the mixed solution that the hydrofluoric acid of the hydrochloric acid of 10-30% and 5-15% is formed carries out pickling, and the weight ratio of hydrochloric acid, hydrofluoric acid is 2-3: 1; After the pickling quartz glass tube is cut, burns mouth, ultrasonic cleaning and deshydroxy and handle, get finished product.
In the production technology scheme of above-described superfine high-purity quartz glass pipe for high-temperature sensor:
1, in step (1), the time of soaking in the raw material input hydrochloric acid is preferably 24 hours.
2, in the mixing acid of step (3), the weight ratio of hydrochloric acid, nitric acid, hydrofluoric acid is preferably 1: 1: 1.
3, in step (4), kerosene, oleic acid, alcoholic acid weight ratio are preferably 1: 1: 1.
4, in step (6), the vacuum tightness when deshydroxy is really handled preferably is not less than 1 * 10
-4, temperature preferably is not less than 1500 ℃, soaking time and is preferably greater than 12 hours.
The metallogenic theory of technological basis quartz of the present invention, comprehensive physics removal of impurities (be generally and adopt artificial naked eyes fine purifiation raw material), chemical purification, high temperature is removed comprehensive purification methods such as gaseous impurities, produces the high-purity ground quartz that meets the product innovation demand.Adopt normal temperature salt acid soak, remove partial impurities; Adopt high-temperature roasting, Water Quenching, carry out high-temperature roasting by the high-temperature roasting stove, under the condition of high temperature, corollary failure quartz raw material intrinsic contaminants structure, make it progressively discharge impurity under the condition of high temperature, quartz raw material is shrend at high temperature, destroys quartzy crystalline structure, make it be easy to fragmentation, the data that instant trace analysis and test quartz raw material reduce through the high-temperature roasting rear impurity.Employing mixing acid soaks, and the multinomial impurity after chemical reaction in the silica powder is progressively reduced.Adopt ultrasonic wave multiple elements chemical medicament high temperature to mix and wash technology, further reduced impurity.Carry out high-temp chlorination and handle, make the impurity that is difficult in acid soak, get rid of, discharge by chloridized.Each treatment step of technology of the present invention complements each other, and interlocks step by step, removes the various impurity in the raw material effectively.
Compared with prior art; the quartz glass tube of explained hereafter of the present invention preparation has ultra-fine, ultra-thinly to be waited to levy; have that high temperature resistant, anti-molten steel and glass metal wash away, corrosion-resistant, heat transfer rate is fast, the soaking performance is good, intensity is big, long service life, technical characterstic such as not explosion under shock heating quenching conditions; technology is workable; but the big production of mass-producing meets the various performance index requirements as pyrostat overcoat pillar fully.
Embodiment
Below further describe concrete technical scheme of the present invention,, and do not constitute restriction its right so that those skilled in the art understands the present invention further.
Embodiment 1.A kind of production technique of superfine high-purity quartz glass pipe for high-temperature sensor, its step is as follows:
(1) optimum break is 20-30mm, SiO
2Content is that the quartz wedge more than 99% is a raw material; With raw material drop into mass percent concentration be soak 40 hours in 10% the hydrochloric acid after, with pure water wash-out hydrochloric acid, until the electric conductivity of wash-out water less than 60us/c m; Get the quartzy material of pickling;
(2) the quartzy material of pickling is dropped in the stoving oven, 850 ℃ of ℃ of following roastings 5 hours, roasting was carried out shrend with pure water after finishing immediately, carries out mechanical disintegration again, sieve 40-140 order silica powder; With high magnetic machine silica powder being carried out deironing then handles;
(3) be to soak 6 days in the mixing acid formed of the hydrofluoric acid of 10% hydrochloric acid, 10% nitric acid and 5% the silica powder input after the deironing by mass percent concentration, the weight ratio of hydrochloric acid, nitric acid, hydrofluoric acid is 1: 2: 1; Soaking the back will soak slurry to be concentrated into concentration be 30% under 40 ℃; Must soak slurry;
(4) will soak slurry drops in the ultrasonoscope, adding the mixed solution of being made up of kerosene, oleic acid and ethanol again carries out high temperature and mixes and wash under 300 ℃ of conditions, the weight of mixed solution is for soaking 15% of slurry weight, mix when washing and regulate pH value to 7.3 with ammoniacal liquor, kerosene, oleic acid, alcoholic acid weight ratio are 1: 2: 1 in the mixed solution; Must mix the pulp washing material;
(5) will mix the pulp washing material and drop in the chlorination reaction still, and carry out high-temp chlorination and handle mixing the pulp washing material under 500 ℃ of conditions, be that 10% hydrochloric acid carried out high-temperature chlorination 2.0 hours by chlorine, tetrachloromethane and mass percent concentration during processing; Dry after the reaction, deironing handles, the magneticstrength of high magnetic machine is 1800KA/m during deironing; Get the glass sand of total impurities content less than 30ppm;
(6) after glass sand drops into and to carry out melting in the quartz continuous melting furnace, be drawn into diameter and be 1.3 quartz glass tube; Get quartz glass tube then, using by mass percent concentration is that the mixed solution that the hydrofluoric acid of 10% hydrochloric acid and 5% is formed carries out pickling, and the weight ratio of hydrochloric acid, hydrofluoric acid is 2: 1; After the pickling quartz glass tube is cut, burns mouth, ultrasonic cleaning and deshydroxy and handle, get finished product.
Embodiment 2.A kind of production technique of superfine high-purity quartz glass pipe for high-temperature sensor, its step is as follows:
(1) optimum break is 20-30mm, SiO
2Content is that the quartz wedge more than 99% is a raw material; With raw material drop into mass percent concentration be soak 20 hours in 30% the hydrochloric acid after, with pure water wash-out hydrochloric acid, until the electric conductivity of wash-out water less than 60us/cm; Get the quartzy material of pickling;
(2) the quartzy material of pickling is dropped in the stoving oven, 900 ℃ of following roastings 3 hours, roasting was carried out shrend with pure water after finishing immediately, carries out mechanical disintegration again, sieve 40-140 order silica powder; With high magnetic machine silica powder being carried out deironing then handles;
(3) be to soak 4 days in the mixing acid formed of the hydrofluoric acid of 30% hydrochloric acid, 30% nitric acid and 15% the silica powder input after the deironing by mass percent concentration, the weight ratio of hydrochloric acid, nitric acid, hydrofluoric acid is 2: 1: 1; Soaking the back will soak slurry to be concentrated into concentration be 45% under 45 ℃; Must soak slurry;
(4) will soak slurry drops in the ultrasonoscope, adding the mixed solution of being made up of kerosene, oleic acid and ethanol again carries out high temperature and mixes and wash under 500 ℃ of conditions, the weight of mixed solution is for soaking 30% of slurry weight, mix when washing and regulate pH value to 7.5 with ammoniacal liquor, kerosene, oleic acid, alcoholic acid weight ratio are 2: 1: 1 in the mixed solution; Must mix the pulp washing material;
(5) will mix the pulp washing material and drop in the chlorination reaction still, and carry out high-temp chlorination and handle mixing the pulp washing material under 1400 ℃ of conditions, be that 30% hydrochloric acid carried out high-temperature chlorination 2.0 hours by chlorine, tetrachloromethane and mass percent concentration during processing; Dry after the reaction, deironing handles, the magneticstrength of high magnetic machine is 2200KA/m during deironing; Get the glass sand of total impurities content less than 30ppm;
(6) after glass sand drops into and to carry out melting in the quartz continuous melting furnace, be drawn into diameter and be 1.5 quartz glass tube; Get quartz glass tube then, using by mass percent concentration is that the mixed solution that the hydrofluoric acid of 30% hydrochloric acid and 15% is formed carries out pickling, and the weight ratio of hydrochloric acid, hydrofluoric acid is 3: 1; After the pickling quartz glass tube is cut, burns mouth, ultrasonic cleaning and deshydroxy and handle, get finished product.
Embodiment 3.A kind of production technique of superfine high-purity quartz glass pipe for high-temperature sensor, its step is as follows:
(1) optimum break is 20-30mm, SiO
2Content is that the quartz wedge more than 99% is a raw material; With raw material drop into mass percent concentration be soak 24 hours in 20% the hydrochloric acid after, with pure water wash-out hydrochloric acid, until the electric conductivity of wash-out water less than 60us/cm; Get the quartzy material of pickling;
(2) the quartzy material of pickling is dropped in the stoving oven, 880 ℃ of following roastings 4 hours, roasting was carried out shrend with pure water after finishing immediately, carries out mechanical disintegration again, sieve 40-140 order silica powder; With high magnetic machine silica powder being carried out deironing then handles;
(3) be to soak 5 days in the mixing acid formed of the hydrofluoric acid of 20% hydrochloric acid, 20% nitric acid and 10% the silica powder input after the deironing by mass percent concentration, the weight ratio of hydrochloric acid, nitric acid, hydrofluoric acid is 1: 1: 1; Soaking the back will soak slurry to be concentrated into concentration be 38% under 42 ℃; Must soak slurry;
(4) will soak slurry drops in the ultrasonoscope, adding the mixed solution of being made up of kerosene, oleic acid and ethanol again carries out high temperature and mixes and wash under 400 ℃ of conditions, the weight of mixed solution is for soaking 22% of slurry weight, mix when washing and regulate pH value to 7.4 with ammoniacal liquor, kerosene, oleic acid, alcoholic acid weight ratio are 1: 1: 1 in the mixed solution; Must mix the pulp washing material;
(5) will mix the pulp washing material and drop in the chlorination reaction still, and carry out high-temp chlorination and handle mixing the pulp washing material under 1000 ℃ of conditions, be that 20% hydrochloric acid carried out high-temperature chlorination 1 hour by chlorine, tetrachloromethane and mass percent concentration during processing; Dry after the reaction, deironing handles, the magneticstrength of high magnetic machine is 2000KA/m during deironing; Get the glass sand of total impurities content less than 30ppm;
(6) after glass sand drops into and to carry out melting in the quartz continuous melting furnace, be drawn into diameter and be 1.4 quartz glass tube; Get quartz glass tube then, using by mass percent concentration is that the mixed solution that the hydrofluoric acid of 20% hydrochloric acid and 10% is formed carries out pickling, and the weight ratio of hydrochloric acid, hydrofluoric acid is 2.5: 1; After the pickling quartz glass tube is cut, burns mouth, ultrasonic cleaning and deshydroxy and handle, get finished product; Vacuum tightness when deshydroxy is really handled is not less than 1 * 10
-4, temperature is not less than 1500 ℃, soaking time greater than 12 hours.
The finished product quartz glass tube of making is detected, and its key technical indexes is as follows: diameter:
(1.4 external diameter) mm; Wall thickness: 0.40mm; The no gas line bubble in surface; Lose circularity less than 0.01mm; Total impurities content: 15ppm; Hydroxy radical content: 3ppm; Good toughness, processability is good, the inwall cleaning.
Claims (5)
1. the production technique of a superfine high-purity quartz glass pipe for high-temperature sensor is characterized in that, its step is as follows:
(1) optimum break is 20-30mm, SiO
2Content is that the quartz wedge more than 99% is a raw material; With raw material drop in the hydrochloric acid that mass percent concentration is 10-30% soak 20-40 hour after, with pure water wash-out hydrochloric acid, until the electric conductivity of wash-out water less than 60us/cm; Get the quartzy material of pickling;
(2) the quartzy material of pickling is dropped in the stoving oven, at 850 ℃ of-900 ℃ of following roasting 3-5 hours, roasting was carried out shrend with pure water after finishing immediately, carries out mechanical disintegration again, sieve 40-140 order silica powder;
With high magnetic machine silica powder being carried out deironing then handles;
(3) be to soak 4-6 days in the mixing acid formed of the hydrofluoric acid of the nitric acid of hydrochloric acid, 10-30% of 10-30% and 5-15% by mass percent concentration with the silica powder input after the deironing, the weight ratio of hydrochloric acid, nitric acid, hydrofluoric acid is 1-2: 1-2: 1-2; Soaking the back will soak slurry to be concentrated into concentration be 30-45% under 40-45 ℃; Must soak slurry;
(4) will soak slurry drops in the ultrasonoscope, adding the mixed solution of being made up of kerosene, oleic acid and ethanol again carries out high temperature and mixes and wash under 300-500 ℃ of condition, the weight of mixed solution is for soaking the 15-30% of slurry weight, mix when washing and regulate the pH value to 7.3-7.5 with ammoniacal liquor, kerosene, oleic acid, alcoholic acid weight ratio are 1-2: 1-2: 1-2 in the mixed solution; Must mix the pulp washing material;
(5) will mix the pulp washing material and drop in the chlorination reaction still, and carry out high-temp chlorination and handle mixing the pulp washing material under 500-1400 ℃ of condition, be that the hydrochloric acid of 10-30% carried out high-temperature chlorination 0.5-2.0 hour by chlorine, tetrachloromethane and mass percent concentration during processing; Dry after the reaction, deironing handles, the magneticstrength of high magnetic machine is 1800-2200KA/m during deironing; Get the glass sand of total impurities content less than 30ppm;
(6) after glass sand drops into and carries out melting in the quartz continuous melting furnace, be drawn into the quartz glass tube that diameter is 1.3-1.5; Get quartz glass tube then, using by mass percent concentration is that the mixed solution that the hydrofluoric acid of the hydrochloric acid of 10-30% and 5-15% is formed carries out pickling, and the weight ratio of hydrochloric acid, hydrofluoric acid is 2-3: 1; After the pickling quartz glass tube is cut, burns mouth, ultrasonic cleaning and deshydroxy and handle, get finished product.
2. the production technique of superfine high-purity quartz glass pipe for high-temperature sensor according to claim 1 is characterized in that, in step (1), it is 24 hours that raw material drops into the time of soaking in the hydrochloric acid.
3. the production technique of superfine high-purity quartz glass pipe for high-temperature sensor according to claim 1, it is characterized in that: in the mixing acid of step (3), the weight ratio of hydrochloric acid, nitric acid, hydrofluoric acid is 1: 1: 1.
4. the production technique of superfine high-purity quartz glass pipe for high-temperature sensor according to claim 1, it is characterized in that: in step (4), kerosene, oleic acid, alcoholic acid weight ratio are 1: 1: 1.
5. the production technique of superfine high-purity quartz glass pipe for high-temperature sensor according to claim 1, it is characterized in that: in step (6), the vacuum tightness when deshydroxy is really handled is not less than 1 * 10
-4, temperature is not less than 1500 ℃, soaking time greater than 12 hours.
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Cited By (8)
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| CN102225838A (en) * | 2011-06-20 | 2011-10-26 | 桂林市光隆光电科技有限公司 | Rotatable temperature control heater |
| CN102981221A (en) * | 2012-12-03 | 2013-03-20 | 连云港市盛昌照明电器有限公司 | Method for manufacturing sleeve for optical fiber connector |
| CN103771708A (en) * | 2014-01-09 | 2014-05-07 | 秦皇岛星箭特种玻璃有限公司 | High-strength display screen glass |
| CN103771689A (en) * | 2014-01-24 | 2014-05-07 | 南通惠通纺织器材有限公司 | Preparation method for high-efficiency and energy-saving electric-power-supply low-hydroxyl-content quartz pipe capable of filtering ultraviolet |
| CN106082238A (en) * | 2016-06-01 | 2016-11-09 | 安徽晶晶石英科技有限公司 | A kind of method of purification of quartz sand |
| CN106186685A (en) * | 2016-07-27 | 2016-12-07 | 连云港福东正佑照明电器有限公司 | A kind of purple quartz tube and preparation method thereof |
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| CN109293225A (en) * | 2018-11-08 | 2019-02-01 | 连云港善发石英制品有限公司 | A kind of production method of thick-walled quartz glass tubes |
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| CN101186455A (en) * | 2007-12-17 | 2008-05-28 | 段其九 | Preparation method of quartz sand used for quartz crucible |
| CN101259963A (en) * | 2008-02-05 | 2008-09-10 | 锦州新世纪石英玻璃有限公司 | Method for producing solar energy stage polycrystalline silicon by using high-pure quartz sand as raw material |
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| CN101186455A (en) * | 2007-12-17 | 2008-05-28 | 段其九 | Preparation method of quartz sand used for quartz crucible |
| CN101259963A (en) * | 2008-02-05 | 2008-09-10 | 锦州新世纪石英玻璃有限公司 | Method for producing solar energy stage polycrystalline silicon by using high-pure quartz sand as raw material |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225838A (en) * | 2011-06-20 | 2011-10-26 | 桂林市光隆光电科技有限公司 | Rotatable temperature control heater |
| CN102981221A (en) * | 2012-12-03 | 2013-03-20 | 连云港市盛昌照明电器有限公司 | Method for manufacturing sleeve for optical fiber connector |
| CN103771708A (en) * | 2014-01-09 | 2014-05-07 | 秦皇岛星箭特种玻璃有限公司 | High-strength display screen glass |
| CN103771689A (en) * | 2014-01-24 | 2014-05-07 | 南通惠通纺织器材有限公司 | Preparation method for high-efficiency and energy-saving electric-power-supply low-hydroxyl-content quartz pipe capable of filtering ultraviolet |
| CN106082238A (en) * | 2016-06-01 | 2016-11-09 | 安徽晶晶石英科技有限公司 | A kind of method of purification of quartz sand |
| CN106186685A (en) * | 2016-07-27 | 2016-12-07 | 连云港福东正佑照明电器有限公司 | A kind of purple quartz tube and preparation method thereof |
| CN106186685B (en) * | 2016-07-27 | 2019-06-28 | 连云港福东正佑照明电器有限公司 | A kind of purple quartz tube and preparation method thereof |
| CN106882918A (en) * | 2017-04-08 | 2017-06-23 | 贵州大学 | Micro-nano nozzle forging instrument apparatus and forging method |
| CN106882918B (en) * | 2017-04-08 | 2023-07-21 | 贵州大学 | Micro-nano nozzle forging instrument and forging method |
| CN109293225A (en) * | 2018-11-08 | 2019-02-01 | 连云港善发石英制品有限公司 | A kind of production method of thick-walled quartz glass tubes |
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Owner name: LIANYUNGANG SHENGCHANG LIGHTING ELECTRIC APPLIANCE Free format text: FORMER OWNER: LI YUSHENG Effective date: 20120618 |
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Effective date of registration: 20120618 Address after: 222300, No. 106 Yingbin Road North, cow town, Donghai County Development Zone, Jiangsu, Lianyungang Patentee after: LIANYUNGANG SHENGCHANG LIGHTING ELECTRICAL APPLIANCES CO., LTD. Address before: 222300, Lianyungang, Jiangsu province Donghai County Yingbin Avenue North Road, 106 Chang Sheng Lighting Appliance Co., Ltd. Patentee before: Li Yusheng |