CN102115095A - Production method of anhydrous ammonium hydrogen fluoride - Google Patents
Production method of anhydrous ammonium hydrogen fluoride Download PDFInfo
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- CN102115095A CN102115095A CN2010106247936A CN201010624793A CN102115095A CN 102115095 A CN102115095 A CN 102115095A CN 2010106247936 A CN2010106247936 A CN 2010106247936A CN 201010624793 A CN201010624793 A CN 201010624793A CN 102115095 A CN102115095 A CN 102115095A
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Abstract
The invention discloses a production method of anhydrous ammonium hydrogen fluoride. The production method comprises the following steps: 1, a neutralization reaction occurs between hydrous hydrofluoric acid or anhydrous hydrofluoric acid and liquid ammonia in a reaction kettle to produce a mixed solution of ammonium fluoride and ammonium hydrogen fluoride; 2, the mixed solution of ammonium fluoride and ammonium hydrogen fluoride is pumped into a concentration tower for vacuum low-temperature concentration so that the concentration of the mixed solution of ammonium fluoride and ammonium hydrogen fluoride reaches more than 70%; 3, the mixed solution of ammonium fluoride and ammonium hydrogen fluoride with the concentration more than 70% is pumped to a high-temperature transformation kettle, and ammonia gas that is decomposed during the transformation process is guided into the reaction kettle for recovery; and 4, a discharge valve of the high-temperature transformation kettle is opened so that the material flow passes through a scraping machine to produce sheet-like anhydrous ammonium hydrogen fluoride. The production method is reasonable in design, has lower requirements for equipment conditions, is easy to promote, and plays a positive role in environmental protection as well as comprehensive resource utilization.
Description
Technical field
The present invention relates to a kind of production method of anhydrous hydrogen fluoride ammonium, belong to chemical production field.
Background technology
External at present production anhydrous hydrogen fluoride ammonium all adopts anhydrous hydrogen fluoride, liquefied ammonia as raw material, earlier with these two kinds of material gasifications, under the gaseous state condition, react, under melting condition, remove unnecessary hydrogen fluoride and ammonia, again through cooling, moulding, make product, its chemical principle is: 2AHF (gas phase)+NH
3(gas phase)-NH
4HF
2The problem of using this method to exist has: 1, must use anhydrous hydrogen fluoride, limited raw material sources, and cost be higher; 2, material removes ammonia, cooling, recovery, moulding through gasification, reaction, defluorination, and technical process is longer, the equipment requirements height, and production capacity is low, the corresponding cost that increased.
Liquid phase method is produced ammonium bifluoride, is to feed liquefied ammonia in water hydrofluoric acid is arranged, or anhydrous hydrogen fluoride fed has made water hydrofluoric acid in the water earlier and feed liquefied ammonia again, through crystallisation by cooling, and centrifuge dehydration, finished product packing.The moisture that contains 3%-5% in the product, can't use in the occasion of having relatively high expectations, and very easily lump, domestic many manufacturers add anti-caking additive, but can influence use for preventing caking in product, if increase baking operation, temperature control is improper, can cause product to decompose, contaminate environment and increase cost; Because of the ammonium bifluoride reaction end of liquid phase method production shows that with pH value product is the mixture of Neutral ammonium fluoride and ammonium bifluoride, its chemical principle is: HF+H
2O+NH
3-NH
4F
2+ NH
4F+H
2O.
Summary of the invention
Purpose of the present invention aims to provide a kind of production method of anhydrous hydrogen fluoride ammonium, the anhydrous hydrogen fluoride ammonium of production, and quality is good, and cost is low, does not lump.
For achieving the above object, the production method of anhydrous hydrogen fluoride ammonium of the present invention may further comprise the steps:
1, with having water hydrofluoric acid or anhydrous hydrogen fluoride and liquefied ammonia to carry out neutralization reaction in reactor, the control pH value is between 3.5-6, and controlled temperature is at 40 ℃--and between 80 ℃, use water quench in the reaction process, generate the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride;
2, the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride is pumped into the upgrading tower still and enter vacuum and low temperature and concentrate, temperature is controlled at 65 ℃--and between 90 ℃, vacuum degree control reaches more than 70% the mixing solutions concentration of Neutral ammonium fluoride and ammonium bifluoride between 0.5-0.95pa;
3, concentration is reached the Neutral ammonium fluoride more than 70% and the mixing solutions of ammonium bifluoride and pump into the pyrolytic conversion still, temperature is controlled at 130 ℃--between 200 ℃, negative pressure is controlled between the 0.4-0.9pa in the still, keeps 10-20 minute, and the ammonia that decomposites in conversion imports reactor and recycles;
4, open the discharging lock of pyrolytic conversion still, streams forms sheet anhydrous hydrogen fluoride ammonium through scraping machine.
The main chemical reactions principle of production method of the present invention is:
1、nHF+H
2O+nNH
3→nNH
4HF
2+nNH
4F+H
2O
2、NH
4HF
2+NH
4F+H
2O→NH
4F+NH
4F
2+H
2O↑
3、2NH
4F→NH
4HF
2+NH
3↑
The production method of anhydrous hydrogen fluoride ammonium of the present invention compared with prior art has following excellent effect:
1, adopt byproduct to have water hydrofluoric acid or anhydrous hydrogen fluoride to do raw material, not only cost is low, has also improved quality product;
2, adopt byproduct to have water hydrofluoric acid or anhydrous hydrogen fluoride to do raw material,, remove most of moisture, enter the pyrolytic conversion still then, under condition of negative pressure, remove unnecessary ammonia element and residual moisture, make the product water content at several ppm through cryoconcentration;
3, the anhydrous hydrogen fluoride ammonium that adopts the inventive method to produce does not lump, and has expanded the scope of application of product;
4, production technique of the present invention is reasonable in design, and appointed condition is less demanding, is easy to promote;
5, to the protection environment, utilize resources synthetically all will play active effect.
Embodiment
Embodiment 1
1, with having water hydrofluoric acid or anhydrous hydrogen fluoride and liquefied ammonia to carry out neutralization reaction in reactor, the control pH value is between 3.5-6, and controlled temperature is at 40 ℃--and between 80 ℃, use water quench in the reaction process, generate the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride;
2, the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride is pumped into the upgrading tower still and enter vacuum and low temperature and concentrate, temperature is controlled at 65 ℃--and between 90 ℃, vacuum degree control reaches more than 70% the mixing solutions concentration of Neutral ammonium fluoride and ammonium bifluoride between 0.5-0.95pa;
3, concentration is reached the Neutral ammonium fluoride more than 70% and the mixing solutions of ammonium bifluoride and pump into the pyrolytic conversion still, temperature is controlled at 130 ℃--between 200 ℃, negative pressure is controlled between the 0.4-0.9pa in the still, keeps 10-20 minute, and the ammonia that decomposites in conversion imports reactor and recycles;
4, open the discharging lock of pyrolytic conversion still, streams forms sheet anhydrous hydrogen fluoride ammonium through scraping machine.
Embodiment 2
1, with having water hydrofluoric acid or anhydrous hydrogen fluoride and liquefied ammonia to carry out neutralization reaction in reactor, the control pH value is between 4.5-5, and controlled temperature is at 50 ℃--and between 70 ℃, use water quench in the reaction process, generate the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride;
2, the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride is pumped into the upgrading tower still and enter vacuum and low temperature and concentrate, temperature is controlled at 70 ℃--and between 85 ℃, vacuum degree control reaches more than 70% the mixing solutions concentration of Neutral ammonium fluoride and ammonium bifluoride between 0.6-0.85pa;
3, concentration is reached the Neutral ammonium fluoride more than 70% and the mixing solutions of ammonium bifluoride and pump into the pyrolytic conversion still, temperature is controlled at 140 ℃--between 190 ℃, negative pressure is controlled between the 0.5-0.8pa in the still, keeps 10-20 minute, and the ammonia that decomposites in conversion imports reactor and recycles;
4, open the discharging lock of pyrolytic conversion still, streams forms sheet anhydrous hydrogen fluoride ammonium through scraping machine.
Embodiment 3
1, with having water hydrofluoric acid or anhydrous hydrogen fluoride and liquefied ammonia to carry out neutralization reaction in reactor, the control pH value is between 4-5.5, and controlled temperature is at 55 ℃--and between 65 ℃, use water quench in the reaction process, generate the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride;
2, the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride is pumped into the upgrading tower still and enter vacuum and low temperature and concentrate, temperature is controlled at 75 ℃--and between 80 ℃, vacuum degree control reaches more than 70% the mixing solutions concentration of Neutral ammonium fluoride and ammonium bifluoride between 0.7-0.8pa;
3, concentration is reached the Neutral ammonium fluoride more than 70% and the mixing solutions of ammonium bifluoride and pump into the pyrolytic conversion still, temperature is controlled at 150 ℃--between 180 ℃, negative pressure is controlled between the 0.6-0.7pa in the still, keeps 10-20 minute, and the ammonia that decomposites in conversion imports reactor and recycles;
4, open the discharging lock of pyrolytic conversion still, streams forms sheet anhydrous hydrogen fluoride ammonium through scraping machine.
Embodiment 4
1, with having water hydrofluoric acid or anhydrous hydrogen fluoride and liquefied ammonia to carry out neutralization reaction in reactor, the control pH value is 3.5, and controlled temperature is used water quench at 40 ℃ in the reaction process, generate the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride;
2, the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride is pumped into the upgrading tower still and enter vacuum and low temperature and concentrate, temperature is controlled at 65 ℃, and vacuum degree control reaches more than 70% the mixing solutions concentration of Neutral ammonium fluoride and ammonium bifluoride at 0.5pa;
3, concentration is reached the Neutral ammonium fluoride more than 70% and the mixing solutions of ammonium bifluoride and pump into the pyrolytic conversion still, temperature is controlled at 130 ℃, and negative pressure is controlled at 0.4pa in the still, keeps 10-20 minute, and the ammonia that decomposites in conversion imports reactor and recycles;
4, open the discharging lock of pyrolytic conversion still, streams forms sheet anhydrous hydrogen fluoride ammonium through scraping machine.
Embodiment 5
1, with having water hydrofluoric acid or anhydrous hydrogen fluoride and liquefied ammonia to carry out neutralization reaction in reactor, the control pH value is 6, and controlled temperature is used water quench at 80 ℃ in the reaction process, generate the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride;
2, the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride is pumped into the upgrading tower still and enter vacuum and low temperature and concentrate, temperature is controlled at 90 ℃, and vacuum degree control reaches more than 70% the mixing solutions concentration of Neutral ammonium fluoride and ammonium bifluoride at 0.95pa;
3, concentration is reached the Neutral ammonium fluoride more than 70% and the mixing solutions of ammonium bifluoride and pump into the pyrolytic conversion still, temperature is controlled at 200 ℃, and negative pressure is controlled at 0.9pa in the still, keeps 10-20 minute, and the ammonia that decomposites in conversion imports reactor and recycles;
4, open the discharging lock of pyrolytic conversion still, streams forms sheet anhydrous hydrogen fluoride ammonium through scraping machine.
Claims (5)
1. the production method of an anhydrous hydrogen fluoride ammonium is characterized in that this method may further comprise the steps:
(1), with having water hydrofluoric acid or anhydrous hydrogen fluoride and liquefied ammonia in reactor, to carry out neutralization reaction, the control pH value is between 3.5-6, controlled temperature is at 40 ℃--between 80 ℃, use water quench in the reaction process, the mixing solutions of generation Neutral ammonium fluoride and ammonium bifluoride;
(2), the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride being pumped into the upgrading tower still enters vacuum and low temperature and concentrates, temperature is controlled at 65 ℃--between 90 ℃, vacuum degree control reaches more than 70% the mixing solutions concentration of Neutral ammonium fluoride and ammonium bifluoride between 0.5-0.95pa;
(3), concentration is reached the Neutral ammonium fluoride more than 70% and the mixing solutions of ammonium bifluoride and pump into the pyrolytic conversion still, temperature is controlled at 130 ℃--between 200 ℃, negative pressure is controlled between the 0.4-0.9pa in the still, keeps 10-20 minute, and the ammonia that decomposites in conversion imports reactor and recycles;
(4), open the discharging lock of pyrolytic conversion still, streams forms sheet anhydrous hydrogen fluoride ammonium through scraping machine.
2. the production method of anhydrous hydrogen fluoride ammonium according to claim 1 is characterized in that
(1) with having water hydrofluoric acid or anhydrous hydrogen fluoride and liquefied ammonia to carry out neutralization reaction in reactor, the control pH value is between 4.5-5, and controlled temperature is at 50 ℃--and between 70 ℃, use water quench in the reaction process, generate the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride;
(2), the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride being pumped into the upgrading tower still enters vacuum and low temperature and concentrates, temperature is controlled at 70 ℃--between 85 ℃, vacuum degree control reaches more than 70% the mixing solutions concentration of Neutral ammonium fluoride and ammonium bifluoride between 0.6-0.85pa;
(3), concentration is reached the Neutral ammonium fluoride more than 70% and the mixing solutions of ammonium bifluoride and pump into the pyrolytic conversion still, temperature is controlled at 140 ℃--between 190 ℃, negative pressure is controlled between the 0.5-0.8pa in the still, keeps 10-20 minute, and the ammonia that decomposites in conversion imports reactor and recycles;
(4), open the discharging lock of pyrolytic conversion still, streams forms sheet anhydrous hydrogen fluoride ammonium through scraping machine.
3. the production method of anhydrous hydrogen fluoride ammonium according to claim 1 is characterized in that
(1), with having water hydrofluoric acid or anhydrous hydrogen fluoride and liquefied ammonia in reactor, to carry out neutralization reaction, the control pH value is between 4-5.5, controlled temperature is at 55 ℃--between 65 ℃, use water quench in the reaction process, the mixing solutions of generation Neutral ammonium fluoride and ammonium bifluoride;
(2), the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride is pumped into the upgrading tower still enter vacuum and low temperature and concentrate, temperature is controlled at 75 ℃--between 80 ℃, vacuum degree control reaches more than 70% the mixing solutions concentration of Neutral ammonium fluoride and ammonium bifluoride between 0.7-0.8pa;
(3), concentration is reached the Neutral ammonium fluoride more than 70% and the mixing solutions of ammonium bifluoride and pump into the pyrolytic conversion still, temperature is controlled at 150 ℃--between 180 ℃, negative pressure is controlled between the 0.6-0.7pa in the still, keeps 10-20 minute, and the ammonia that decomposites in conversion imports reactor and recycles;
(4), open the discharging lock of pyrolytic conversion still, streams forms sheet anhydrous hydrogen fluoride ammonium through scraping machine.
4. the production method of anhydrous hydrogen fluoride ammonium according to claim 1 is characterized in that
(1), with having water hydrofluoric acid or anhydrous hydrogen fluoride and liquefied ammonia in reactor, to carry out neutralization reaction, the control pH value is 3.5, controlled temperature use water quench at 40 ℃ in the reaction process, the mixing solutions of generation Neutral ammonium fluoride and ammonium bifluoride;
(2), the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride is pumped into the upgrading tower still enter vacuum and low temperature and concentrate, temperature is controlled at 65 ℃, vacuum degree control reaches more than 70% the mixing solutions concentration of Neutral ammonium fluoride and ammonium bifluoride at 0.5pa;
(3), concentration is reached Neutral ammonium fluoride more than 70% and the mixing solutions of ammonium bifluoride pumps into the pyrolytic conversion still, temperature is controlled at 130 ℃, negative pressure is controlled at 0.4pa in the still, keeps 10-20 minute, the ammonia that decomposites in conversion imports reactor and recycles;
(4), open the discharging lock of pyrolytic conversion still, streams forms sheet anhydrous hydrogen fluoride ammonium through scraping machine.
5. the production method of anhydrous hydrogen fluoride ammonium according to claim 1 is characterized in that
(1), with having water hydrofluoric acid or anhydrous hydrogen fluoride and liquefied ammonia in reactor, to carry out neutralization reaction, the control pH value is 6, controlled temperature use water quench at 80 ℃ in the reaction process, the mixing solutions of generation Neutral ammonium fluoride and ammonium bifluoride;
(2), the mixing solutions of Neutral ammonium fluoride and ammonium bifluoride is pumped into the upgrading tower still enter vacuum and low temperature and concentrate, temperature is controlled at 90 ℃, vacuum degree control reaches more than 70% the mixing solutions concentration of Neutral ammonium fluoride and ammonium bifluoride at 0.95pa;
(3), concentration is reached Neutral ammonium fluoride more than 70% and the mixing solutions of ammonium bifluoride pumps into the pyrolytic conversion still, temperature is controlled at 200 ℃, negative pressure is controlled at 0.9pa in the still, keeps 10-20 minute, the ammonia that decomposites in conversion imports reactor and recycles;
(4), open the discharging lock of pyrolytic conversion still, streams forms sheet anhydrous hydrogen fluoride ammonium through scraping machine.
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|---|---|---|---|
| CN201010624793.6A CN102115095B (en) | 2010-12-31 | 2010-12-31 | Production method of anhydrous ammonium hydrogen fluoride |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539156A (en) * | 2013-10-23 | 2014-01-29 | 衢州市鼎盛化工科技有限公司 | Preparation method of anhydrous ammonium hydrogen fluoride and micro-channel reaction device thereof |
| CN104140113A (en) * | 2014-07-15 | 2014-11-12 | 浙江工业大学 | Method for preparing anti-blocking ammonium bifluoride |
| CN106044796A (en) * | 2016-06-29 | 2016-10-26 | 福建天福化工有限公司 | Preparation method of high-purity flaky ammonium bifluoride |
| CN108793192A (en) * | 2018-08-20 | 2018-11-13 | 福建永晶科技股份有限公司 | A kind of preparation method and its preparation system of ammonium fluoride |
| CN108910916A (en) * | 2018-08-20 | 2018-11-30 | 福建永晶科技股份有限公司 | A kind of preparation method and its preparation system of ammonium acid fluoride |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385369A (en) * | 2002-01-15 | 2002-12-18 | 姜仁和 | Proces for direct synthesizing fluoammonium salt |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385369A (en) * | 2002-01-15 | 2002-12-18 | 姜仁和 | Proces for direct synthesizing fluoammonium salt |
Non-Patent Citations (1)
| Title |
|---|
| 曹宏伟等: "氟化氢铵生产新工艺研究", 《磷肥与复肥》, vol. 25, no. 4, 31 July 2010 (2010-07-31) * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539156A (en) * | 2013-10-23 | 2014-01-29 | 衢州市鼎盛化工科技有限公司 | Preparation method of anhydrous ammonium hydrogen fluoride and micro-channel reaction device thereof |
| CN104140113A (en) * | 2014-07-15 | 2014-11-12 | 浙江工业大学 | Method for preparing anti-blocking ammonium bifluoride |
| CN104140113B (en) * | 2014-07-15 | 2016-02-24 | 浙江工业大学 | A kind of preparation method of anti-caking ammonium bifluoride |
| CN106044796A (en) * | 2016-06-29 | 2016-10-26 | 福建天福化工有限公司 | Preparation method of high-purity flaky ammonium bifluoride |
| CN108793192A (en) * | 2018-08-20 | 2018-11-13 | 福建永晶科技股份有限公司 | A kind of preparation method and its preparation system of ammonium fluoride |
| CN108910916A (en) * | 2018-08-20 | 2018-11-30 | 福建永晶科技股份有限公司 | A kind of preparation method and its preparation system of ammonium acid fluoride |
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| CN102115095B (en) | 2014-05-14 |
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