CN1899658A - Method for preparing gas purifying agent for simultaneously removing trace oxygen and trace water in inert gas - Google Patents
Method for preparing gas purifying agent for simultaneously removing trace oxygen and trace water in inert gas Download PDFInfo
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- CN1899658A CN1899658A CN 200610200712 CN200610200712A CN1899658A CN 1899658 A CN1899658 A CN 1899658A CN 200610200712 CN200610200712 CN 200610200712 CN 200610200712 A CN200610200712 A CN 200610200712A CN 1899658 A CN1899658 A CN 1899658A
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- oxygen
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- water
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- purifying agent
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Abstract
The present invention belongs to the field of functional inorganic material preparing technology, and is preparation process of granular inorganic purifying agent material for simultaneously eliminating trace oxygen and trace water in inert gas. The present invention features that one kind of supported active oxygen and water eliminating purifying agent is prepared by means of oxidation reduction and active adsorption principle and filled to the filler column for eliminating oxygen and water from inert gas out of steel cylinder completely. The present invention can meet the requirement of no water and no oxygen operation in different fields.
Description
Technical field
The invention belongs to the functional inorganic materials preparing technical field, specially refer to a kind of inorganic cleanser granular materials preparation method who removes trace water and trace oxygen in the noble gas simultaneously.
Background technology
In many real processes such as organic synthesis, analytical test, electronic welding and processing or the packing of product, often run into noble gas and do protective gas or do the situation of carrier gas.The effect of noble gas is done the diluent in analyzing at some, and prior function is anti-locking system and airborne water and/or oxygen generation chemical reaction.But, contain more or less minor amount of water and oxygen in all gases of existing market supply all the time.Find in the application, even the high pure nitrogen that use in the laboratory is not also got rid of the interference of oxygen and water fully.In many cases, the existence of this trace constituent can cause side reaction generation, product to decompose even produce blast etc.At present about trace water in the noble gas and oxygen to deviate from method more loaded down with trivial details and complicated, many reactions or operation can not be carried out or be maintained on the certain level because of the limitation of conditions.For this reason, this patent provides a kind of simple and easy inorganic cleanser preparation method who removes trace oxygen and water in the noble gas, can make that oxygen and water content are reduced to zero simultaneously in the noble gas.
Summary of the invention
The purpose of this invention is to provide a kind of low cost, simply remove the inorganic cleanser method of trace oxygen and water in the noble gas, can make that oxygen and water content are reduced to zero simultaneously in the noble gas, thereby satisfy specific demands such as Chemical Manufacture, scientific research and high-tech area.
Technical scheme of the present invention is to utilize redox and activated adoption reaction principle, with iron, copper, manganese, antimony metal salt and silicon, aluminum oxide is raw material, getting wherein one or more carries out chemical reaction and generates a kind of loaded deoxidation dehydration predecessor granular materials, this material is put in the filled column, after reduction is handled, formed highly active collaborative deoxidation dehydration granular filler.When the gas that comes out from steel cylinder passed through this filled column, oxygen was consumed by high reducing metal compound activity component in the filler; Chemical reaction and suction-operated also take place and are removed fully under this active component catalysis in water simultaneously.Therefore make the oxygen G﹠W in the noble gas be reduced to zero.This filler will become dark-brown from green behind inactivation, reuse after regenerating.
Effect of the present invention and benefit are: a kind of method for gas purification that simply removes trace oxygen and water in the noble gas is provided, can have made that oxygen and water are reduced to zero in the gas.This technology is grasped easily and is applied.The present invention shows obvious competitive advantages and profit margin at aspects such as manufacturing cost, properties of product and environmental friendliness.
The specific embodiment
Be described in detail the specific embodiment of the present invention and step below in conjunction with technical scheme.
The inorganic cleanser granular materials preparation method who removes trace water and trace oxygen in the noble gas of the present invention is characterized in that cleanser composition of raw materials, formula rate and particle size are as follows:
The metal active composition is chosen in chloride, nitrate, sulfate or the acetate of Fe, Cu, Mn, Sb metal in the cleanser raw material, can be wherein one or more; Loaded sorbing material is at SiO
2Or Al
2O
3Or choose in their hydrate, can be wherein a kind of or whole; The weight concentration of Fe, Cu, Mn, Sb slaine changes in 10 ~ 70%; Supporting the absorbing material granules size changes in 40 ~ 200 orders; Fe, Cu, Mn, Sb slaine and the weight ratio that supports oxide are 1: 100 ~ 3: 1.The technological process of technology of preparing is as follows:
Step 1: will support hydrochloric acid or the nitric acid washing of sorbing material, and filter and place it in the baking oven dry down then in 120 ~ 200 ℃ with 0.05 ~ 2M;
Step 2: metal salt solution chosen and join in the scope of formula concentration and ratio regulation support in the sorbing material, then they be placed in the baking oven in 120 ~ 200 ℃ down baking till supporting the sorbing material blackening;
Step 3: the material after step 2 oven dry packed into one to be had in the long glass tube of heating jacket, glass tube is become green (changing into of color be black → palm fibre → green) being heated to 350 ~ 450 ℃ of materials in whole glass tube under the situation that constantly has hydrogen stream to cross, continue logical argon gas/nitrogen several hours then to drive remaining water away under 450 ℃ in glass tube, this green matter is gas purifying agent;
Step 4: during use, will pass through above-mentioned glass filler post by gas dry and deoxidation, and flow through in the process of filled column at gas, wherein moisture and oxygen are removed simultaneously;
Step 5: when the cleanser in the glass column lost efficacy, that is: become when brown or coffee-like from green, repeating step 2 makes its regeneration.In order to guarantee the deaerating effect that dewaters of this device, answer to be in barotropic state in the assurance device all the time, general not exclusively close the noble gas valve, but the time spent must not connect all the valve closing of giving vent to anger of instruments.It should be noted that in order to prevent the air suck-back, blast pipe is inserted in below the mercury face.
Embodiment 1
With 60 ~ 150 purpose Al
2O
3Or SiO
2With 0.1 ~ 1.0M salt acid elution, filter and place it in the baking oven dry down then in 150 ~ 200 ℃; With weight concentration 10 ~ 50% Cu (NO
3)
2Or Mn (NO
3)
2Solution is by 50 ~ 100ml/100g Al
2O
3(or SiO
2) ratio join Al
2O
3In, they are placed in the baking oven toast until Al down then in 150-200 ℃
2O
3(SiO
2) till the blackening, note in drying course, having poisonous NO
2Emit with NO gas; Material after the oven dry is packed into one and had in the long glass tube of heating jacket, glass tube is become green being heated to 400 ~ 450 ℃ of materials in whole glass tube under the situation that constantly has hydrogen stream to cross, under 450 ℃, in glass tube, continue logical argon gas/nitrogen several hours then to drive remaining water away; Will pass through above-mentioned glass filler post by gas dry and deoxidation during use, outlet oxygen G﹠W is wherein promptly removed fully.
Claims (1)
1. gas purifying agent preparation method who removes trace oxygen and trace water in the noble gas simultaneously is characterized in that cleanser composition of raw materials, formula rate and particle size are as follows:
The metal active composition is chosen in chloride, nitrate, sulfate or the acetate of Fe, Cu, Mn, Sb metal in the cleanser raw material, is wherein one or more; Loaded sorbing material is chosen in SiO2 or Al2O3 or their hydrate, is wherein a kind of or whole; The weight concentration of Fe, Cu, Mn, Sb slaine changes in 10 ~ 70%; Supporting the absorbing material granules size changes in 40 ~ 200 orders; Fe, Cu, Mn, Sb slaine and the weight ratio that supports oxide are 1: 100 ~ 3: 1; The technological process of technology of preparing is as follows:
Step 1: will support hydrochloric acid or the nitric acid washing of sorbing material, and filter and place it in the baking oven dry down then in 120 ~ 200 ℃ with 0.05 ~ 2M;
Step 2: metal salt solution chosen and join in the scope of formula concentration and ratio regulation support in the sorbing material, then they are placed in the baking oven in 120 ~ 200 ℃ of bakings down, till supporting the sorbing material blackening;
Step 3: the material after step 2 oven dry packed into one to be had in the long glass tube of heating jacket, glass tube is become green (changing into of color be black → palm fibre → green) being heated to 350 ~ 450 ℃ of materials in whole glass tube under the situation that constantly has hydrogen stream to cross, continue logical argon gas/nitrogen several hours then to drive remaining water away under 450 ℃ in glass tube, this green matter is gas purifying agent;
Step 4: during use, will pass through above-mentioned glass filler post by gas dry and deoxidation, and flow through in the process of filled column at gas, wherein moisture and oxygen are removed simultaneously;
Step 5: when the cleanser in the glass column lost efficacy, that is: become when brown or coffee-like from green, repeating step 2 makes its regeneration; In order to guarantee the deaerating effect that dewaters of this device, answer to be in barotropic state in the assurance device all the time, general not exclusively close the noble gas valve, but the time spent must not connect all the valve closing of giving vent to anger of instruments; It should be noted that in order to prevent the air suck-back, blast pipe is inserted in below the mercury face.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006102007123A CN100409916C (en) | 2006-07-21 | 2006-07-21 | Method for preparing gas purifying agent for simultaneously removing trace oxygen and trace water in inert gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006102007123A CN100409916C (en) | 2006-07-21 | 2006-07-21 | Method for preparing gas purifying agent for simultaneously removing trace oxygen and trace water in inert gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1899658A true CN1899658A (en) | 2007-01-24 |
| CN100409916C CN100409916C (en) | 2008-08-13 |
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ID=37655761
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006102007123A Expired - Fee Related CN100409916C (en) | 2006-07-21 | 2006-07-21 | Method for preparing gas purifying agent for simultaneously removing trace oxygen and trace water in inert gas |
Country Status (1)
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|---|---|
| CN (1) | CN100409916C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627026A (en) * | 2019-09-10 | 2019-12-31 | 东南大学 | Online purification method for removing trace combustible gas in inert gas |
-
2006
- 2006-07-21 CN CNB2006102007123A patent/CN100409916C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627026A (en) * | 2019-09-10 | 2019-12-31 | 东南大学 | Online purification method for removing trace combustible gas in inert gas |
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| Publication number | Publication date |
|---|---|
| CN100409916C (en) | 2008-08-13 |
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Granted publication date: 20080813 Termination date: 20110721 |