CN102275951A - Method for producing super-pure ammonia water - Google Patents
Method for producing super-pure ammonia water Download PDFInfo
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- CN102275951A CN102275951A CN 201010195268 CN201010195268A CN102275951A CN 102275951 A CN102275951 A CN 102275951A CN 201010195268 CN201010195268 CN 201010195268 CN 201010195268 A CN201010195268 A CN 201010195268A CN 102275951 A CN102275951 A CN 102275951A
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Abstract
The invention relates to a method for producing super-pure ammonia water, which comprises: gasifying liquid ammonia water, introducing ammonia gas into an ultrasonic wave purifying tower, wherein the ultrasonic wave purifying tower is provided with an ultrasonic wave atomizer and super-pure water, and the ultrasonic wave atomizer generates fine ammonia water particles to absorb the impurities in the ammonia gas; and filtering obtained pure ammonia gas by a filter and delivering the pure ammonia gas to a product absorbing tower to combine the ammonia gas with super-pure water in the product absorbing tower, and thus, obtaining super-pure ammonia water. Compared with the prior art, the method is suitable for producing super-pure ammonia water product and industrial ammonia water product serving as byproduct. The super-pure ammonia water product prepared by the method meet the following indexes: the ammonia water content is more than or equal to 28 percent; the single negative ion impurity content is less than or equal to 10ppb; the single positive ion impurity content is less than or equal to 0.1ppb; the industrial ammonia water content is more than or equal to 28 percent; the process is safe and reliable; the equipment structure is compact; the energy consumption is low; the production is free discharge of waste water, water gas and water residue; and the method meets the environment-protection requirement.
Description
Technical field
The present invention relates to a kind of method of producing ammoniacal liquor, especially relate to a kind of method of producing ultrapure ammoniacal liquor.
Background technology
The aquatic product of ultra-pure ammonia has the multistage distillation method, absorbs desorption method etc., but not all ionic impurity can both with aforesaid method be purified or can be economical reach desired degree of purification.The product that produces with multistage distillation method or absorption desorption method production impurity≤0.1ppb as the purification of sodium, arsonium ion impurity has bigger high energy consumption and danger, and it is huge to absorb the desorption method facility investment, and distillation method high-temperature operation process is brought potential safety hazard again.In order to solve the defective that exists on the prior art, and this technological invention of exploitation has high quality, less energy-consumption, the feature of environmental protection, safety advantages.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of process safety reliable for the defective that overcomes above-mentioned prior art existence, compact equipment, less energy-consumption, the method for the ultrapure ammoniacal liquor of production of three-waste free discharge.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of method of producing ultrapure ammoniacal liquor, it is characterized in that, this method may further comprise the steps: import the ultrasonic purification tower with the liquid ammonia gasification and with ammonia, this ultrasonic purification tower bottom is provided with ultrasonic atomizer, ultrapure water is housed in the ultrasonic atomizer, this ultrasonic atomizer produces trickle ammoniacal liquor particle, utilize the impurity in the trickle ammoniacal liquor particle absorbing ammonia, the purifying ammonia that obtains enters the product absorption tower after device filters after filtration, and this ammonia combines with ultrapure water in the product absorption tower and obtains ultrapure ammoniacal liquor.
Temperature in the described ultrasonic purification tower is 0～50 ℃, and pressure is 0.08～0.8MPa.
Described ultrasonic purification tower adds pre-treatment medicaments, and described pre-treatment medicaments is ammonium persulphate, hydrogen peroxide or phosphoric acid.
The add-on of described pre-treatment medicaments is by 0.01～1% of the ammonia weight of ultrasonic purification tower.
Described trickle ammoniacal liquor particle combines with the part ammonia behind ultrasonic atomizer atomizing ultrapure water and obtains, and the particle diameter of trickle ammoniacal liquor particle is 0.1～30 μ m.
Described trickle ammoniacal liquor particle is 1 with weight ratio by ultrasonic purification tower ammonia: (10～300).
Temperature in the described product absorption tower is 0～50 ℃, and pressure is 0.04～0.6MPa.
In addition, the concentration 〉=28wt% of described ammoniacal liquor, single anion impurity≤10ppb, single cation impurity≤0.1ppb.
Fail to be entered waste gas absorption tower and carry out the terminal absorption combines the formation lower concentration with pure water ammoniacal liquor, and mix formation technical grade ammoniacal liquor product with the high density ammoniacal liquor of regular discharging in the ultrasonic purification tower by the small amount of ammonia gas that the product absorption tower absorbs fully.
Temperature in the described waste gas absorption tower is 0～50 ℃, and pressure is 0.01～0.4MPa.
Compared with prior art, the present invention is fit to production ultra-pure ammonia fishery products, simultaneously by-product technical grade ammoniacal liquor product.Adopt gained ultra-pure ammonia fishery products of the present invention to meet following index: ammoniacal liquor content 〉=28%, single anion impurity≤10ppb, single cation impurity≤0.1ppb.Technical grade ammoniacal liquor content 〉=28%, process safety is reliable, compact equipment, three-waste free discharge is produced in less energy-consumption simultaneously, satisfies environmental requirement.
Description of drawings
Fig. 1 is a schema of the present invention among the embodiment 1.
1 is that ammonia liquor container, 2 is that ultrasonic purification tower, 3 is that ultrasonic atomizer, 4 is that strainer, 5 is that product absorption tower, 6 is that waste gas absorption tower, 7 is that ultra-pure ammonia water collecting device, 8 is a technical grade ammoniacal liquor collection device among the figure.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
A kind of method of producing ultrapure ammoniacal liquor, its flow process as shown in Figure 1, this method may further comprise the steps:
The ammonia that volatilization in the ammonia liquor container 1 forms is imported in the ultrasonic purification tower 2, ultrasonic purification tower temperature is controlled to be 〉=and 0 ℃, pressure-controlling is 〉=0.08Mpa, add pre-treatment medicaments ammonium persulphate targetedly toward ultrasonic purification tower 2, the ammonium persulphate add-on is that it is volatile to the influential impurity of end product quality to be used for the complexing ammonia by 0.01% of the ammonia weight of ultrasonic purification tower.In ultrasonic purification tower 2, produce a large amount of trickle ammoniacal liquor particles by ultrasonic atomizer 3, the ammoniacal liquor particle diameter distributes substantially at 0.1～30 μ m, ammoniacal liquor particle generation is 1: 300 with ammonia weight ratio by the ultrasonic purification tower, utilizes the surface-area of a large amount of trickle ammoniacal liquor particle flood tides to absorb contained more impurity in the ammonia.The ammoniacal liquor particle that the effect of the purifying ammonia that obtains by strainer 4 will contain more impurity filters to be held back, make the ammonia that obtains purifying be able to by.The ammonia of purifying enters product absorption tower 5, the temperature on product absorption tower 5 is controlled to be 〉=and 0 ℃, pressure-controlling is 〉=0.04Mpa, by forming the ultra-pure ammonia fishery products with combining of product absorption tower 5 interior ultrapure waters, ammoniacal liquor content 〉=28%, single anion impurity≤10ppb, single cation impurity≤0.1ppb, ultrapure ammoniacal liquor is collected in the ultra-pure ammonia water collecting device 7.Fail to be entered waste gas absorption tower 6 by the small amount of ammonia gas that product absorption tower 5 absorbs fully, the temperature of waste gas absorption tower 6 is controlled to be 〉=and 0 ℃, pressure-controlling is 〉=0.01Mpa, carry out terminal and absorb the ammoniacal liquor that combines the formation lower concentration with pure water, mix back ammoniacal liquor content 〉=28% with the high density ammoniacal liquor that discharges in the ultrasonic purification tower, form technical grade ammoniacal liquor product, be collected in the technical grade ammoniacal liquor collection device 8.
A kind of method of producing ultrapure ammoniacal liquor, this method may further comprise the steps:
The ammonia that volatilization in the ammonia liquor container forms is imported in the ultrasonic purification tower, ultrasonic purification tower temperature is controlled to be 20 ℃, pressure-controlling is 0.3Mpa, add pre-treatment medicaments hydrogen peroxide targetedly toward the ultrasonic purification tower, the hydrogen peroxide add-on is that it is volatile to the influential impurity of end product quality to be used for the complexing ammonia by 0.1% of the ammonia weight of ultrasonic purification tower.In the ultrasonic purification tower, produce a large amount of trickle ammoniacal liquor particles by ultrasonic atomizer, the ammoniacal liquor particle diameter distributes substantially at 0.1～30 μ m, ammoniacal liquor particle generation is 1: 150 with ammonia weight ratio by the ultrasonic purification tower, utilizes the surface-area of a large amount of trickle ammoniacal liquor particle flood tides to absorb contained more impurity in the ammonia.The ammoniacal liquor particle that the effect of the purifying ammonia that obtains by strainer will contain more impurity filters to be held back, make the ammonia that obtains purifying be able to by.The ammonia of purifying enters the product absorption tower, the temperature on product absorption tower is controlled to be 20 ℃, pressure-controlling is 0.2Mpa, by with the product absorption tower in combining of ultrapure water form the ultra-pure ammonia fishery products, ammoniacal liquor content 〉=28%, single anion impurity≤10ppb, single cation impurity≤0.1ppb, ultrapure ammoniacal liquor is collected in the ultra-pure ammonia water collecting device.Fail to be entered waste gas absorption tower by the small amount of ammonia gas that the product absorption tower absorbs fully, the temperature of waste gas absorption tower is controlled to be 20 ℃, pressure-controlling is 0.1Mpa, carry out terminal and absorb the ammoniacal liquor that combines the formation lower concentration with pure water, mix back ammoniacal liquor content 〉=28% with the high density ammoniacal liquor that discharges in the ultrasonic purification tower, form technical grade ammoniacal liquor product, be collected in the technical grade ammoniacal liquor collection device.
A kind of method of producing ultrapure ammoniacal liquor, this method may further comprise the steps:
The ammonia that volatilization in the ammonia liquor container forms is imported in the ultrasonic purification tower, ultrasonic purification tower temperature is controlled to be≤and 50 ℃, pressure-controlling is≤0.8Mpa, add pre-treatment medicaments phosphoric acid targetedly toward the ultrasonic purification tower, the phosphoric acid add-on is that it is volatile to the influential impurity of end product quality to be used for the complexing ammonia by 1% of the ammonia weight of ultrasonic purification tower.In the ultrasonic purification tower, produce a large amount of trickle ammoniacal liquor particles by ultrasonic atomizer, the ammoniacal liquor particle diameter distributes substantially at 0.1～30 μ m, ammoniacal liquor particle generation is 1: 10 with ammonia weight ratio by the ultrasonic purification tower, utilizes the surface-area of a large amount of trickle ammoniacal liquor particle flood tides to absorb contained more impurity in the ammonia.The ammoniacal liquor particle that the effect of the purifying ammonia that obtains by strainer will contain more impurity filters to be held back, make the ammonia that obtains purifying be able to by.The ammonia of purifying enters the product absorption tower, the temperature on product absorption tower is controlled to be≤and 50 ℃, pressure-controlling is≤0.6Mpa, by with the product absorption tower in combining of ultrapure water form the ultra-pure ammonia fishery products, ammoniacal liquor content 〉=28%, single anion impurity≤10ppb, single cation impurity≤0.1ppb, ultrapure ammoniacal liquor is collected in the ultra-pure ammonia water collecting device.Fail to be entered waste gas absorption tower by the small amount of ammonia gas that the product absorption tower absorbs fully, the temperature of waste gas absorption tower is controlled to be≤and 50 ℃, pressure-controlling is≤0.4Mpa, carry out terminal and absorb the ammoniacal liquor that combines the formation lower concentration with pure water, mix back ammoniacal liquor content 〉=28% with the high density ammoniacal liquor that discharges in the ultrasonic purification tower, form technical grade ammoniacal liquor product, be collected in the technical grade ammoniacal liquor collection device.
Claims (7)
1. method of producing ultrapure ammoniacal liquor, it is characterized in that, this method may further comprise the steps: import the ultrasonic purification tower with the liquid ammonia gasification and with ammonia, this ultrasonic purification tower bottom is provided with ultrasonic atomizer, ultrapure water is housed in the ultrasonic atomizer, this ultrasonic atomizer produces trickle ammoniacal liquor particle, utilize the impurity in the trickle ammoniacal liquor particle absorbing ammonia, the purifying ammonia that obtains enters the product absorption tower after device filters after filtration, and this ammonia combines with ultrapure water in the product absorption tower and obtains ultrapure ammoniacal liquor.
2. a kind of method of producing ultrapure ammoniacal liquor according to claim 1 is characterized in that, the temperature in the described ultrasonic purification tower is 0～50 ℃, and pressure is 0.08～0.8MPa.
3. a kind of method of producing ultrapure ammoniacal liquor according to claim 1 is characterized in that, described ultrasonic purification tower adds pre-treatment medicaments, and described pre-treatment medicaments is ammonium persulphate, hydrogen peroxide or phosphoric acid.
4. a kind of method of producing ultrapure ammoniacal liquor according to claim 3 is characterized in that, the add-on of described pre-treatment medicaments is by 0.01～1% of the ammonia weight of ultrasonic purification tower.
5. a kind of method of producing ultrapure ammoniacal liquor according to claim 1 is characterized in that, described trickle ammoniacal liquor particle combines with the part ammonia behind ultrasonic atomizer atomizing ultrapure water and obtains, and the particle diameter of trickle ammoniacal liquor particle is 0.1～30 μ m.
6. a kind of method of producing ultrapure ammoniacal liquor according to claim 1 is characterized in that, described trickle ammoniacal liquor particle is 1 with weight ratio by ultrasonic purification tower ammonia: (10～300).
7. a kind of method of producing ultrapure ammoniacal liquor according to claim 1 is characterized in that the temperature in the described product absorption tower is 0～50 ℃, and pressure is 0.04～0.6MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010195268 CN102275951A (en) | 2010-06-08 | 2010-06-08 | Method for producing super-pure ammonia water |
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| CN 201010195268 CN102275951A (en) | 2010-06-08 | 2010-06-08 | Method for producing super-pure ammonia water |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105954348A (en) * | 2016-07-19 | 2016-09-21 | 株洲科能新材料有限责任公司 | Analysis and detection method for high purity indium |
| CN114432855A (en) * | 2022-02-16 | 2022-05-06 | 内蒙古新雨稀土功能材料有限公司 | A equipment system for synthesizing high-purity carbonic acid rare earth precipitant |
| CN115159543A (en) * | 2022-06-29 | 2022-10-11 | 镇江润晶高纯化工科技股份有限公司 | High-purity ammonia water preparation process capable of continuously preparing and reducing use energy consumption |
| CN115504486A (en) * | 2022-09-20 | 2022-12-23 | 湖北兴福电子材料股份有限公司 | Production method of ultra-pure electronic grade ammonia water |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996039265A1 (en) * | 1995-06-05 | 1996-12-12 | Startec Ventures, Inc. | On-site ammonia purification for semiconductor manufacture |
| CN1300634A (en) * | 2000-11-16 | 2001-06-27 | 上海哈勃化工有限公司 | Process for preparing super-impurity chemical |
| CN1335259A (en) * | 2000-07-28 | 2002-02-13 | 日本派欧尼股份株式会社 | Process for purifying ammonia |
-
2010
- 2010-06-08 CN CN 201010195268 patent/CN102275951A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996039265A1 (en) * | 1995-06-05 | 1996-12-12 | Startec Ventures, Inc. | On-site ammonia purification for semiconductor manufacture |
| CN1335259A (en) * | 2000-07-28 | 2002-02-13 | 日本派欧尼股份株式会社 | Process for purifying ammonia |
| CN1300634A (en) * | 2000-11-16 | 2001-06-27 | 上海哈勃化工有限公司 | Process for preparing super-impurity chemical |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105954348A (en) * | 2016-07-19 | 2016-09-21 | 株洲科能新材料有限责任公司 | Analysis and detection method for high purity indium |
| CN105954348B (en) * | 2016-07-19 | 2018-05-22 | 株洲科能新材料有限责任公司 | A kind of Analysis of High-Purity Indium detection method |
| CN114432855A (en) * | 2022-02-16 | 2022-05-06 | 内蒙古新雨稀土功能材料有限公司 | A equipment system for synthesizing high-purity carbonic acid rare earth precipitant |
| CN115159543A (en) * | 2022-06-29 | 2022-10-11 | 镇江润晶高纯化工科技股份有限公司 | High-purity ammonia water preparation process capable of continuously preparing and reducing use energy consumption |
| CN115504486A (en) * | 2022-09-20 | 2022-12-23 | 湖北兴福电子材料股份有限公司 | Production method of ultra-pure electronic grade ammonia water |
| CN115504486B (en) * | 2022-09-20 | 2024-03-12 | 湖北兴福电子材料股份有限公司 | Production method of ultra-high-purity electronic grade ammonia water |
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Application publication date: 20111214 |