CN102861560A - Modification method of electronic gas absorbent - Google Patents
Modification method of electronic gas absorbent Download PDFInfo
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- CN102861560A CN102861560A CN2012104045873A CN201210404587A CN102861560A CN 102861560 A CN102861560 A CN 102861560A CN 2012104045873 A CN2012104045873 A CN 2012104045873A CN 201210404587 A CN201210404587 A CN 201210404587A CN 102861560 A CN102861560 A CN 102861560A
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Abstract
The invention relates to a modification method of an absorbent, particularly relates to a modification method of an electronic gas absorbent and solves the problem that existing electronic gas absorbents are low in absorbing amount. The modification method includes firstly, placing the electronic gas absorbent in an absorber to be heated; and secondly, feeding a mixture gas of hydrogen and trimethyl aluminum steam into the absorber from an inlet at an uniform speed and discharging the mixture gas from an outlet at a speed which is the same as the speed at which the mixture gas is fed. According to the modification method of the electronic gas absorbent, trimethyl aluminum is used as load metal to modify activated carbon, zeolite and silica gel, the absorbing capacity is enhanced after modification, and the absorption amount is increased by 25-40%. The modification method of the electronic gas absorbent is applied to the field of micro-electronics.
Description
Technical field
The present invention relates to the method for modifying of adsorbent.
Background technology
High pure electronic gas is one of backing material of microelectronic industry, make computer chip, large scale integrated circuit, also have the electronic device of the aspects such as Aero-Space all to be unable to do without high pure electronic gas, particularly in many important sophisticated technology fields, all must use gaseous mass to be the high pure electronic gas more than the 6N.The employed high pure electronic gas of China all depends on import at present, has greatly restricted the development of China in the high-end technology field, and causes product cost high.And high pure electronic gas can be used for the anticorrosion of the preparation of semiconductor integrated circuit N-type and grain.
But through containing a large amount of oxygen and moisture in the electronic gas of purifying, do not limited its application, so need before use electronic gas is carried out purifying.With adsorbent wherein impurity being adsorbed is a kind of very practical and economic method.But be subject to the impact of the aspects such as the structure of adsorbent and performance, the adsorbance of adsorbent is low, and the adsorbance that the adsorbance that is generally 18g/mL, active carbon such as the adsorbance of zeolite is generally 25g/mL, silica gel is generally 5g/mL.So, need under normal conditions adsorbent is carried out modification.
Summary of the invention
The present invention is the low problem of adsorbance that will solve existing electronic gas adsorbent, and a kind of method of modifying of electronic gas adsorbent is provided.
The method of modifying of a kind of electronic gas adsorbent of the present invention carries out: one, the electronic gas adsorbent is inserted in the absorber and heat according to the following steps; Wherein, described electronic gas adsorbent is zeolite, silica gel or active carbon; The heating-up temperature of zeolite and active carbon is 550～700 ℃, and be 1.5～3h heat time heating time; The heating-up temperature of silica gel is 150～220 ℃, and be 1.5～3h heat time heating time;
The volume ratio of two, pressing hydrogen and trimethyl aluminium steam is (6～7): (3～4), at the uniform velocity pass into the mist of hydrogen and trimethyl aluminium steam from the porch to absorber, and to discharge mist with the same speed that passes into mist from the exit, the time that passes into of mist is 1.5～4h, and the intake of mist is: the volume of the used mist of every 1t electronic gas adsorbent is 180～500L;
The present invention utilizes the adsorptivity of adsorbent, adsorbing metal ions at first on adsorbent surface, the reproducibility of recycling adsorbent, metal ion is reduced into the ion of simple substance or lower valency, by metal or metal ion the stronger adhesion of adsorbed material is increased adsorbent to the absorption property of adsorbed material.The present invention uses trimethyl aluminium as carried metal, and to active carbon, zeolite, and silica gel carries out modification, and adsorption capacity has obtained enhancing after the modification, and adsorbance has improved 25～40%.
The specific embodiment
The specific embodiment one: the method for modifying of a kind of electronic gas adsorbent of present embodiment is to carry out according to the following steps: one, the electronic gas adsorbent is inserted in the absorber and heat; Wherein, described electronic gas adsorbent is zeolite, silica gel or active carbon; The heating-up temperature of zeolite and active carbon is 550～700 ℃, and be 1.5～3h heat time heating time; The heating-up temperature of silica gel is 150～220 ℃, and be 1.5～3h heat time heating time;
The volume ratio of two, pressing hydrogen and trimethyl aluminium steam is (6～7): (3～4), at the uniform velocity pass into the mist of hydrogen and trimethyl aluminium steam from the porch to absorber, and to discharge mist with the same speed that passes into mist from the exit, the time that passes into of mist is 1.5～4h, and the intake of mist is: the volume of the used mist of every 1t electronic gas adsorbent is 180～500L;
Present embodiment is utilized the adsorptivity of adsorbent, adsorbing metal ions at first on adsorbent surface, the reproducibility of recycling adsorbent, metal ion is reduced into the ion of simple substance or lower valency, by metal or metal ion the stronger adhesion of adsorbed material is increased adsorbent to the absorption property of adsorbed material.The present invention uses trimethyl aluminium as carried metal, and to active carbon, zeolite, and silica gel carries out modification, and adsorption capacity has obtained enhancing after the modification, and adsorbance has improved 25～40%.
The specific embodiment two: what present embodiment and the specific embodiment one were different is, the heating-up temperature of step 1 mesolite and active carbon is 600 ℃, and be 2h heat time heating time.Other is identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different from the specific embodiment one or two is, the heating-up temperature of silica gel is 200 ℃ in the step 1, and be 2h heat time heating time.Other is identical with the specific embodiment one or two.
The specific embodiment four: what present embodiment was different from one of specific embodiment one to three is that the volume ratio of hydrogen and trimethyl aluminium steam is 2: 1 in the step 2.Other is identical with one of specific embodiment one to three.
The specific embodiment five: what present embodiment was different from one of specific embodiment one to four is that the time that passes into of mist is 2h in the step 2.Other is identical with one of specific embodiment one to four.
The specific embodiment six: what present embodiment was different from one of specific embodiment one to five is that the intake of mist is in the step 2: the volume of the used mist of every 1t electronic gas adsorbent is 200L.Other is identical with one of specific embodiment one to five.
By following verification experimental verification beneficial effect of the present invention:
Test the method for modifying of 1 one kinds of electronic gas adsorbents, carry out according to the following steps: one, the halogenation na-pretreated zeolite is inserted and heat in the absorber; Wherein, heating-up temperature is 600 ℃, and be 2h heat time heating time.
Two, the volume ratio by hydrogen and trimethyl aluminium steam is 2: 1, at the uniform velocity pass into the mist of hydrogen and trimethyl aluminium steam from the porch to absorber, and to discharge mist with the same speed that passes into mist from the exit, the time that passes into of mist is 2h, and the intake of mist is: the volume of the used mist of every 1t electronic gas adsorbent is 200L;
Sending into oxygen content in the absorber is 1 * 10
-4The argon of %, dew-point temperature are-50～-60 ℃.The consumption of argon is 1m
3/ t.Oxygen content in the argon of absorber exit is 5 * 10
-7%, the dew-point temperature of argon is subzero-100～-110 ℃.The adsorbance of testing the electronic gas adsorbent of this test preparation by gravimetric method is 25.2g/mL, and the halogenation na-pretreated zeolite before the modification is 18g/mL in the adsorbance of equal conditions.
Test the method for modifying of 2 one kinds of electronic gas adsorbents, carry out according to the following steps: one, the birch active carbon is inserted and heat in the absorber; Wherein, heating-up temperature is 600 ℃, and be 2h heat time heating time.
Two, the volume ratio by hydrogen and trimethyl aluminium steam is 2: 1, at the uniform velocity pass into the mist of hydrogen and trimethyl aluminium steam from the porch to absorber, and to discharge mist with the same speed that passes into mist from the exit, the time that passes into of mist is 2h, and the intake of mist is: the volume of the used mist of every 1t electronic gas adsorbent is 200L;
Sending into oxygen content in the absorber is 1 * 10
-4The hydrogen of %, dew-point temperature are-60～-70 ℃.The oxygen content in absorber exit is 3 * 10
-7%, dew-point temperature is-95～-105 ℃.The adsorbance of testing the electronic gas adsorbent of this test preparation by gravimetric method is 31g/mL, and the birch active carbon before the modification is 25g/mL in the adsorbance of equal conditions.
Test the method for modifying of 3 one kinds of electronic gas adsorbents, carry out according to the following steps: one, silica gel is inserted and heat in the absorber; Wherein, heating-up temperature is 200 ℃, and be 2h heat time heating time.
Two, the volume ratio by hydrogen and trimethyl aluminium steam is 2: 1, at the uniform velocity pass into the mist of hydrogen and trimethyl aluminium steam from the porch to absorber, and to discharge mist with the same speed that passes into mist from the exit, the time that passes into of mist is 2h, and the intake of mist is: the volume of the used mist of every 1t electronic gas adsorbent is 200L;
Send into hydrogen in absorber, wherein the oxygen content of hydrogen is 1 * 10
-4%, dew-point temperature is subzero 60-80 ℃.The oxygen content in absorber exit is 4 * 10
-7%, dew-point temperature is subzero 90-120 ℃.The adsorbance of testing the electronic gas adsorbent of this test preparation by gravimetric method is 30g/mL, and the silica gel before the modification is 5g/mL in the adsorbance of equal conditions.
Claims (6)
1. the method for modifying of an electronic gas adsorbent is characterized in that the method for modifying of electronic gas adsorbent carries out according to the following steps:
One, the electronic gas adsorbent is inserted in the absorber heats; Wherein, described electronic gas adsorbent is zeolite, silica gel or active carbon; The heating-up temperature of zeolite and active carbon is 550～700 ℃, and be 1.5～3h heat time heating time; The heating-up temperature of silica gel is 150～220 ℃, and be 1.5～3h heat time heating time;
The volume ratio of two, pressing hydrogen and trimethyl aluminium steam is (6～7): (3～4), at the uniform velocity pass into the mist of hydrogen and trimethyl aluminium steam from the porch to absorber, and to discharge mist with the same speed that passes into mist from the exit, the time that passes into of mist is 1.5～4h, and the intake of mist is: the volume of the used mist of every 1t electronic gas adsorbent is 180～500L.
2. the method for modifying of a kind of electronic gas adsorbent according to claim 1, the heating-up temperature that it is characterized in that step 1 mesolite and active carbon is 600 ℃, be 2h heat time heating time.
3. the method for modifying of a kind of electronic gas adsorbent according to claim 1, the heating-up temperature that it is characterized in that silica gel in the step 1 is 200 ℃, be 2h heat time heating time.
4. the method for modifying of a kind of electronic gas adsorbent according to claim 1 is characterized in that the volume ratio of hydrogen and trimethyl aluminium steam is 2: 1 in the step 2.
5. the method for modifying of a kind of electronic gas adsorbent according to claim 1 is characterized in that the time that passes into of mist is 2h in the step 2.
6. the method for modifying of a kind of electronic gas adsorbent according to claim 1, it is characterized in that the intake of mist in the step 2 is: the volume of the used mist of every 1t electronic gas adsorbent is 200L.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4554141A (en) * | 1984-05-14 | 1985-11-19 | Ethyl Corporation | Gas stream purification |
| CN1753720A (en) * | 2002-12-26 | 2006-03-29 | 马西森三气公司 | Method and system for supplying high purity fluid |
| CN101342478A (en) * | 2008-08-15 | 2009-01-14 | 王少志 | Purification adsorption agent for silicone hydride, phosphorane, arsine or borane gases and preparation method thereof |
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- 2012-10-22 CN CN2012104045873A patent/CN102861560A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4554141A (en) * | 1984-05-14 | 1985-11-19 | Ethyl Corporation | Gas stream purification |
| CN1753720A (en) * | 2002-12-26 | 2006-03-29 | 马西森三气公司 | Method and system for supplying high purity fluid |
| CN101342478A (en) * | 2008-08-15 | 2009-01-14 | 王少志 | Purification adsorption agent for silicone hydride, phosphorane, arsine or borane gases and preparation method thereof |
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Application publication date: 20130109 |