CN112520699A - Synthetic purification method of arsine - Google Patents
Synthetic purification method of arsine Download PDFInfo
- Publication number
- CN112520699A CN112520699A CN202011385329.6A CN202011385329A CN112520699A CN 112520699 A CN112520699 A CN 112520699A CN 202011385329 A CN202011385329 A CN 202011385329A CN 112520699 A CN112520699 A CN 112520699A
- Authority
- CN
- China
- Prior art keywords
- control module
- central control
- preset
- arsine gas
- arsine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
- C01B6/065—Hydrides of arsenic or antimony
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/34—Purification; Stabilisation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0009—Physical processing
- C01B2210/0014—Physical processing by adsorption in solids
- C01B2210/0015—Physical processing by adsorption in solids characterised by the adsorbent
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0009—Physical processing
- C01B2210/0014—Physical processing by adsorption in solids
- C01B2210/0015—Physical processing by adsorption in solids characterised by the adsorbent
- C01B2210/002—Other molecular sieve materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0042—Making ultrapure specific gas
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0043—Impurity removed
- C01B2210/0051—Carbon dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0043—Impurity removed
- C01B2210/0062—Water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0043—Impurity removed
- C01B2210/0098—Other impurities
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention relates to a synthetic purification method of arsine, which comprises the following steps: the method comprises the following steps: putting zinc powder and arsenic powder into a quartz vessel, uniformly mixing, putting into a stainless steel reaction tank, vacuumizing, filling high-purity inert gas, and pressurizing and heating to obtain zinc arsenide powder; secondly, putting zinc arsenide powder into a reactor, and adding dilute sulfuric acid to react to generate crude arsine gas; step three, introducing the crude arsine gas into an adsorption device to obtain arsine gas; collecting arsine gas by using a liquid nitrogen cold trap, condensing the arsine gas into liquid arsine, pumping out non-condensable gas by using a vacuum pump, taking down a liquid nitrogen tank outside a cold hydrazine, and volatilizing the arsine to obtain pure arsine gas; step five: introducing the pure arsine gas into a clean steel cylinder which is pretreated for storage to obtain a finished product. The method can effectively reduce impurities in arsine gas, improve the purity of arsine, and improve the reaction efficiency by putting the addition of the adsorbent and the selection of the molecular sieve in one device.
Description
Technical Field
The invention relates to the technical field of arsine synthesis, in particular to a method for synthesizing and purifying arsine.
Background
Arsine is one of the five elements of great importance in electronic gases, an important electronic specialty gas, and is used mainly in the semiconductor industry for N-type doping of epitaxial silicon, N-type diffusion in silicon, ion implantation, growth of gallium arsenide and gallium arsenide phosphide, and the like. Furthermore, arsine has very important applications in optoelectronics, solar cells and micro-blogging devices.
Arsine cannot be synthesized simply by simple substances, but arsine can be obtained in the presence of a catalyst or under plasma irradiation, and some metal arsenides are generally used for preparing arsine by reacting with water or acid, wherein the reaction is rapid and complete, hydrogen is completely absent in the product, but the yield of arsine is generally lower than 90%.
Currently, the concentration of arsine prepared by the international advanced level is 6N, while one of the special gases in China, the purity of arsine can only produce standard special gas with the concentration of 3-4N due to technical reasons, and in many important fields, such as: the 6N standard gas urgently needed in the aspects of national war preparedness weapon research, manufacturing of electronic components of a control system on a Shenzhou five carrier rocket, manufacturing of solar cells used on a satellite and the like is imported, only developed countries such as America, Russia and the like can produce the gas in the world at present, and the gas imported in China is usually hindered due to international situation tension and change, so the development of the related fields is directly restrained by the localization problem of continuous high-purity gas materials in China.
The existing domestic arsine purification method is also published, and mainly adopts gallium-indium alloy liquid to deeply adsorb dehydration and oxygen to obtain electronic grade arsine, however, the adsorption mode is not reproducible, and heavy metals are difficult to obtain, so that the cost of the whole system is high, the popularization is limited, and on the other hand, the heavy metal alloys have toxicity and the adsorption efficiency of deep adsorption is low.
Disclosure of Invention
Therefore, the invention provides a method for synthesizing and purifying arsine with high purity, fast reaction and less impurities, which can effectively solve the technical problems in the prior art.
In order to achieve the above object, the present invention provides a method for synthesizing and purifying arsine, comprising:
the method comprises the following steps: putting zinc powder and arsenic powder which are proportioned in advance into a quartz vessel, uniformly mixing, then putting into a stainless steel reaction tank after uniform mixing, vacuumizing, filling high-purity inert gas, and pressurizing and heating to obtain zinc arsenide powder for later use;
step two, putting the zinc arsenide powder collected in the step one into a reactor, and adding dilute sulfuric acid while stirring by using a stirrer to react to generate crude arsine gas;
step three, introducing the crude arsine gas obtained in the step two into an adsorption device, wherein an alkaline porous adsorbent and a molecular sieve are arranged in the adsorption device, so as to obtain arsine gas;
step four, trapping arsine gas in the step three by using a liquid nitrogen cold trap, condensing the arsine gas into liquid arsine, pumping out non-condensable gas by using a vacuum pump, taking down a liquid nitrogen tank outside the cold trap, and volatilizing the arsine to obtain pure arsine gas;
step five: introducing the arsine gas purified in the step five into a clean steel cylinder which is pretreated for storage to obtain a finished product;
the adsorption device and the liquid nitrogen tank are wirelessly connected with the central control module, the central control module is used for controlling the reaction process in the adsorption device, and a matrix is arranged in the central control module;
in the third step, the density of the arsine gas is periodically detected by using a density detector, the central control module calculates the comprehensive density of the arsine gas according to the density of the arsine gas periodically detected and compares the comprehensive density of the arsine gas with the preset comprehensive density of the arsine gas, and if the central control module judges that the comparison result meets a first preset condition, the next step is carried out; if the central control module judges that the comparison result does not accord with the first preset condition, the central control module calculates the arsine gas comprehensive density difference value and matches the arsine gas comprehensive density difference value with the parameters in a preset arsine gas comprehensive density difference value interval matrix delta rho 0, and if the central control module judges that the matching result accords with the second preset condition according to the matching result, the central control module controls a first regulating valve to add the adsorbent; if the central control module judges that the comparison result does not meet a second preset condition, the central control module controls a second regulating valve to select molecular sieves with other specifications;
the central control module establishes an arsine gas density matrix rho (rho 1, rho 2, rho 3, …, rho n) according to the arsine gas density periodically detected by the density monitor, wherein rho 1 represents the arsine gas density detected in the first detection period, rho 2 represents the arsine gas density detected in the second detection period, rho 3 represents the arsine gas density detected in the third detection period, and rho n represents the arsine gas density detected in the nth detection period, and is used for calculating the comprehensive density rhoz of the arsine gas, and the calculation formula is as follows:
ρz=(ρ1+ρ2+ρ3+…+ρn)/(n×α）；
wherein n represents n detection periods, and alpha represents an arsine gas density coefficient;
the central control module is provided with a preset arsine gas comprehensive density rho 0 for comparing with an arsine gas comprehensive density rho z:
if the rho z is not more than rho 0, the central control module tray bottom comparison result meets a first preset condition, and entering the next step;
and if the rho z is larger than the rho 0, the central control module judges that the comparison result does not meet a first preset condition.
Further, the central control module is further provided with a preset arsine gas comprehensive density difference interval matrix delta rho 0 (delta rho 1 and delta rho 2), wherein the delta rho 1 represents a first difference interval of the preset arsine gas comprehensive density, the delta rho 2 represents a second difference interval of the preset arsine gas comprehensive density, and the numerical ranges of the intervals are not overlapped;
when the central control module judges that the comparison result does not meet a first preset condition, the central control module calculates the comprehensive density difference value delta rhoz of the arsine gas and matches the comprehensive density difference value delta rhoz with parameters in a preset comprehensive density difference value interval matrix delta rho 0 of the arsine gas:
if the delta rhoz is within the range of the delta rho 1, the central control module judges that the matching result meets a second preset condition and controls the first regulating valve to add the adsorbent;
if the delta rhoz is within the range of the delta rho 2, the central control module judges that the matching result does not meet a second preset condition and controls a second regulating valve to select molecular sieves with other specifications;
the calculation formula of the arsine gas comprehensive density difference delta rhoz is as follows:
△ρz=（ρz-ρ0）×β；
wherein beta represents the arsine gas integrated density difference coefficient.
Further, the central control module is further provided with a preset arsine gas pH value matrix PH0 (PH 1, PH2, PH3 and PH 4), wherein PH1 represents a first preset arsine gas pH value, PH2 represents a second preset arsine gas pH value, PH3 represents a third preset arsine gas pH value, PH4 represents a fourth preset arsine gas pH value, PH1 is greater than PH2, PH3 is greater than PH 4;
the central control module is further provided with a preset adsorbent adding matrix Mx (Mx1, Mx2, Mx3 and Mx4), wherein Mx1 represents a first adsorbent adding amount, Mx2 represents a second adsorbent adding amount, Mx3 represents a third adsorbent adding amount, and Mx4 represents a fourth adsorbent adding amount;
when the central control module judges that the matching result meets a second preset condition, the central control module controls the arsine gas to be introduced into the pH value detector so as to detect the pH value of the arsine gas and compares the measured pH value PH of the arsine gas with parameters in a preset arsine gas pH value matrix PH 0:
if the PH is less than PH4, the central control module judges that the comparison result meets a third preset condition and further compares the PH with a matrix PH0, and if the PH is less than PH1, the central control module controls a first regulating valve to add an Mx1 amount of adsorbent; if the PH is not less than 1 and is less than 2, the central control module controls the first regulating valve to add the adsorbent with the amount of Mx 2; if the PH is not less than 2 and is less than 3, the central control module controls the first regulating valve to add the adsorbent with the amount of Mx 3; if the PH is not less than 3 and is less than 4, the central control module controls the first regulating valve to add the adsorbent with the amount of Mx 4;
and if the PH is greater than or equal to the PH4, the central control module judges that the comparison result does not meet a third preset condition.
Further, the central control module is further provided with a preset sulfide content matrix S0 (S1, S2, S3, S4), wherein S1 represents a preset sulfide first content, S2 represents a preset sulfide second content, S3 represents a preset sulfide third content, and S4 represents a preset sulfide fourth content;
when the central control module judges that the comparison result does not meet a third preset condition, the central control module controls the arsine gas to be introduced into a sulfide detector to detect the sulfide content of the arsine gas and compares the detected sulfide content S with the parameters in a preset sulfide content matrix S0:
if S = Si, i =1,2,3,4, the central control module controls the first regulating valve to add Myi amounts of adsorbent, Myi = Mxi × η, where η represents an adsorbent adjustment coefficient and Mxi represents a value corresponding to a parameter in the preset adsorbent addition matrix Mx.
Further, the central control module is further provided with a preset carbon dioxide content difference interval matrix deltaC 0 (deltaC 1, deltaC 2, deltaC 3 and deltaC 4), wherein deltaC 1 represents a first difference interval of the preset carbon dioxide content, deltaC 2 represents a second difference interval of the preset carbon dioxide content, deltaC 3 represents a third difference interval of the preset carbon dioxide content, and deltaC 4 represents a fourth difference interval of the preset carbon dioxide content, and the numerical ranges of the intervals are not overlapped;
the central control module is also provided with a preset molecular sieve specification matrix Q0(Q1, Q2, Q3 and Q4), wherein Q1 represents a molecular sieve with the specification of 3A, Q2 represents a molecular sieve with the specification of 4A, Q3 represents a molecular sieve with the specification of 5A, and Q4 represents a molecular sieve with the specification of 13A;
the central control module is also provided with a preset carbon dioxide content C0;
when the central control module judges that the comparison result does not meet a second preset condition, the central control module controls the arsine gas to be introduced into the carbon dioxide content detection device to detect the carbon dioxide content of the arsine gas and compares the detected carbon dioxide content C with a preset carbon dioxide content C0:
if C is less than or equal to C0, the central control module judges that the comparison result meets a fourth preset condition, which indicates that the content of carbon dioxide meets the standard;
if C is more than C0, the central control module judges that the comparison result does not meet a fourth preset condition and calculates the carbon dioxide content difference value delta C, delta C = C-C0, after the calculation is finished, the central control module matches the delta C with the parameters in a preset carbon dioxide content difference value interval matrix delta C0,
if the deltaC is in the deltaC 1 range, the central control module controls the second regulating valve to simultaneously select 1 molecular sieve with the specification of Q1 and 2 molecular sieves with the specification of Q2;
if the deltaC is in the deltaC 2 range, the central control module controls the second regulating valve to simultaneously select 2 molecular sieves with the specification of Q2 and 3 molecular sieves with the specification of Q3;
if the deltaC is in the deltaC 3 range, the central control module controls the second regulating valve to simultaneously select 3 molecular sieves with the specification of Q3 and 1 molecular sieve with the specification of Q4;
if the deltaC is in the deltaC 4 range, the central control module controls the second regulating valve to simultaneously select 3 molecular sieves with the specification of Q1 and 2 molecular sieves with the specification of Q4.
Further, the central control module is further provided with a preset water vapor content matrix H0 (H1, H2, H3, H4), wherein H1 represents a first preset water vapor content, H2 represents a second preset water vapor content, H3 represents a third preset water vapor content, and H4 represents a fourth preset water vapor content;
when the central control module judges that the comparison result does not meet a second preset condition, the central control module controls the arsine gas to be introduced into the humidity meter so as to detect the water vapor content of the arsine gas and compares the detected water vapor content H with the parameters in a preset water vapor content matrix H0:
if H = Hi, i =1,2,3,4, the central control module controls the second regulating valve to select the molecular sieve with the Qi specification, where Qi represents the molecular sieve corresponding to the parameters in the preset molecular sieve specification matrix Q0.
Further, the central control module is also provided with a preset molecular sieve selection coefficient matrix phi 0 (phi 1, phi 2, phi 3, phi 4), wherein phi 1 represents a first preset molecular sieve selection coefficient, phi 2 represents a second preset molecular sieve selection coefficient, phi 3 represents a third preset molecular sieve selection coefficient, and phi 4 represents a fourth preset molecular sieve selection coefficient;
the parameters in the preset water vapor content matrix H0 meet the conditions that H1 is more than H2 is more than H3 is more than H4;
when the central control module judges that the comparison result does not meet a fourth preset condition and selects the molecular sieve according to the matching relationship between the carbon dioxide content difference value and the parameters in the preset carbon dioxide content difference value interval matrix Delta C0, the central control module compares the measured water vapor content H with the parameters in the preset water vapor content matrix H0 and selects the molecular sieve according to the comparison result and the comparison result of the molecular sieve selection coefficient phi and the parameters in the preset molecular sieve selection coefficient matrix phi 0:
when H is less than H1, if phi = phi i, i =1,2,3,4, the central control module controls the second regulating valve to simultaneously select 1 molecular sieve with the specification of Q1 and 1 molecular sieve with the specification of Q2;
when H1 is not less than H < H2, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 2 molecular sieves with the specifications of Q2 and Q3;
when H2 is not less than H < H3, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 3 molecular sieves with the specifications of Q3 and Q4;
when H3 is not less than H < H4, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 4 molecular sieves with the specifications of Q1 and Q4;
when H is larger than or equal to H4, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 1Q 1, 2Q 2, 3Q 3 and 4Q 4 molecular sieves;
the calculation formula of the molecular sieve selection coefficient phi is as follows:
Φ=(H/Hi)/δ;
wherein, Hi represents the steam content corresponding to the parameters in the preset steam content matrix H0, δ represents the molecular sieve adjusting coefficient, i =1,2,3, 4.
Further, the high purity inert gas may be one of high purity helium, neon, argon or nitrogen.
Further, the molecular sieve is an activated alumina silica gel molecular sieve.
Further, the basic porous adsorbent comprises calcium oxide and sodium oxide.
Compared with the prior art, the method has the beneficial effects that the density of the arsine gas is periodically detected by using the density detector, the central control module calculates the comprehensive density of the arsine gas according to the density of the arsine gas periodically detected and compares the comprehensive density with the preset comprehensive density of the arsine gas, and if the central control module judges that the comparison result meets the first preset condition, the next step is carried out; if the central control module judges that the comparison result does not meet the first preset condition, the central control module calculates the arsine gas comprehensive density difference value and matches the arsine gas comprehensive density difference value with the parameters in the preset arsine gas comprehensive density difference value interval matrix delta rho 0, and if the central control module judges that the matching result meets the second preset condition according to the matching result, the central control module controls the first regulating valve to add the adsorbent; if the central control module judges that the comparison result does not meet the second preset condition, the central control module controls the second regulating valve to select the molecular sieves with other specifications, so that acidic substances and sulfides in the arsine gas can be reduced by controlling the first regulating valve to add the adsorbent, carbon dioxide and water vapor in the arsine gas can be reduced by controlling the second regulating valve to select the molecular sieves with other specifications, impurities in the arsine gas can be effectively reduced, the purity of the arsine is improved, and meanwhile, the addition of the adsorbent and the selection of the molecular sieves are carried out in one device, so that the reaction efficiency can be improved.
Drawings
FIG. 1 is a schematic flow diagram of the process for the synthetic purification of arsine according to the invention.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described below with reference to examples; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and do not limit the scope of the present invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Referring to fig. 1, which is a schematic flow chart of the method for synthesizing and purifying arsine according to the present invention, the present invention provides a method for synthesizing and purifying arsine, including:
the method comprises the following steps: putting zinc powder and arsenic powder which are proportioned in advance into a quartz vessel, uniformly mixing, then putting into a stainless steel reaction tank after uniform mixing, vacuumizing, filling high-purity inert gas, and pressurizing and heating to obtain zinc arsenide powder for later use;
step two, putting the zinc arsenide powder collected in the step one into a reactor, and adding dilute sulfuric acid while stirring by using a stirrer to react to generate crude arsine gas;
step three, introducing the crude arsine gas obtained in the step two into an adsorption device, wherein an alkaline porous adsorbent and a molecular sieve are arranged in the adsorption device, so as to obtain arsine gas;
step four, trapping arsine gas in the step three by using a liquid nitrogen cold trap, condensing the arsine gas into liquid arsine, pumping out non-condensable gas by using a vacuum pump, taking down a liquid nitrogen tank outside the cold trap, and volatilizing the arsine to obtain pure arsine gas;
step five: introducing the arsine gas purified in the step five into a clean steel cylinder which is pretreated for storage to obtain a finished product;
the adsorption device and the liquid nitrogen tank are wirelessly connected with the central control module, the central control module is used for controlling the reaction process in the adsorption device, and a matrix is arranged in the central control module;
in the third step, the density of the arsine gas is periodically detected by using a density detector, the central control module calculates the comprehensive density of the arsine gas according to the density of the arsine gas periodically detected and compares the comprehensive density of the arsine gas with the preset comprehensive density of the arsine gas, and if the central control module judges that the comparison result meets a first preset condition, the next step is carried out; if the central control module judges that the comparison result does not accord with the first preset condition, the central control module calculates the arsine gas comprehensive density difference value and matches the arsine gas comprehensive density difference value with the parameters in a preset arsine gas comprehensive density difference value interval matrix delta rho 0, and if the central control module judges that the matching result accords with the second preset condition according to the matching result, the central control module controls a first regulating valve to add the adsorbent; if the central control module judges that the comparison result does not meet a second preset condition, the central control module controls a second regulating valve to select molecular sieves with other specifications;
the central control module establishes an arsine gas density matrix rho (rho 1, rho 2, rho 3, …, rho n) according to the arsine gas density periodically detected by the density monitor, wherein rho 1 represents the arsine gas density detected in the first detection period, rho 2 represents the arsine gas density detected in the second detection period, rho 3 represents the arsine gas density detected in the third detection period, and rho n represents the arsine gas density detected in the nth detection period, and is used for calculating the comprehensive density rhoz of the arsine gas, and the calculation formula is as follows:
ρz=(ρ1+ρ2+ρ3+…+ρn)/(n×α）；
wherein n represents n detection periods, and alpha represents an arsine gas density coefficient;
the central control module is provided with a preset arsine gas comprehensive density rho 0 for comparing with an arsine gas comprehensive density rho z:
if the rho z is not more than rho 0, the central control module tray bottom comparison result meets a first preset condition, and entering the next step;
and if the rho z is larger than the rho 0, the central control module judges that the comparison result does not meet a first preset condition.
In the embodiment of the invention, the arsenic powder and the zinc powder are mixed according to the mass ratio of 3: 4; the pressure is maintained at 0.13-0.14 MPa, and the heating is carried out for 3-4 h; the mass concentration of the dilute sulfuric acid is 10-50%; the heating temperature in the first step is 600-620 ℃; the alkaline porous adsorbent is a porous adsorbent formed by mixing calcium oxide and sodium oxide in a mass ratio of 96: 4; the condensation temperature is-200 to-100 ℃.
In the embodiment of the invention, the density of the arsine gas is periodically detected by using a density detector, the central control module calculates the comprehensive density of the arsine gas according to the periodically detected density of the arsine gas and compares the comprehensive density with the preset comprehensive density of the arsine gas, and if the central control module judges that the comparison result meets a first preset condition, the next step is carried out; if the central control module judges that the comparison result does not meet the first preset condition, the central control module calculates the arsine gas comprehensive density difference value and matches the arsine gas comprehensive density difference value with the parameters in the preset arsine gas comprehensive density difference value interval matrix delta rho 0, and if the central control module judges that the matching result meets the second preset condition according to the matching result, the central control module controls the first regulating valve to add the adsorbent; if the central control module judges that the comparison result does not meet the second preset condition, the central control module controls the second regulating valve to select the molecular sieves with other specifications, so that acidic substances and sulfides in the arsine gas can be reduced by controlling the first regulating valve to add the adsorbent, carbon dioxide and water vapor in the arsine gas can be reduced by controlling the second regulating valve to select the molecular sieves with other specifications, impurities in the arsine gas can be effectively reduced, the purity of the arsine is improved, and meanwhile, the addition of the adsorbent and the selection of the molecular sieves are carried out in one device, so that the reaction efficiency can be improved.
Specifically, the central control module is further provided with a preset arsine gas comprehensive density difference interval matrix delta rho 0 (delta rho 1 and delta rho 2), wherein the delta rho 1 represents a first difference interval of the preset arsine gas comprehensive density, the delta rho 2 represents a second difference interval of the preset arsine gas comprehensive density, and the numerical ranges of the intervals are not overlapped;
when the central control module judges that the comparison result does not meet a first preset condition, the central control module calculates the comprehensive density difference value delta rhoz of the arsine gas and matches the comprehensive density difference value delta rhoz with parameters in a preset comprehensive density difference value interval matrix delta rho 0 of the arsine gas:
if the delta rhoz is within the range of the delta rho 1, the central control module judges that the matching result meets a second preset condition and controls the first regulating valve to add the adsorbent;
if the delta rhoz is within the range of the delta rho 2, the central control module judges that the matching result does not meet a second preset condition and controls a second regulating valve to select molecular sieves with other specifications;
the calculation formula of the arsine gas comprehensive density difference delta rhoz is as follows:
△ρz=（ρz-ρ0）×β；
wherein beta represents the arsine gas integrated density difference coefficient.
According to the embodiment of the invention, the comprehensive density difference value of the arsine gas is matched with the parameters in the preset arsine gas comprehensive density difference value interval matrix delta rho 0, and according to the matching result, the central control module controls the first regulating valve to add the adsorbent or controls the second regulating valve to select the molecular sieves of other specifications, so that acidic substances and sulfides in the arsine gas can be reduced by controlling the first regulating valve to add the adsorbent, carbon dioxide and water vapor in the arsine gas can be reduced by controlling the second regulating valve to select the molecular sieves of other specifications, impurities in the arsine gas can be effectively reduced, and the purity of the arsine is improved.
Specifically, the central control module is further provided with a preset arsine gas pH value matrix PH0 (PH 1, PH2, PH3 and PH 4), wherein PH1 represents a first preset arsine gas pH value, PH2 represents a second preset arsine gas pH value, PH3 represents a third preset arsine gas pH value, PH4 represents a fourth preset arsine gas pH value, PH1 is greater than PH2, PH3 is greater than PH 4;
the central control module is further provided with a preset adsorbent adding matrix Mx (Mx1, Mx2, Mx3 and Mx4), wherein Mx1 represents a first adsorbent adding amount, Mx2 represents a second adsorbent adding amount, Mx3 represents a third adsorbent adding amount, and Mx4 represents a fourth adsorbent adding amount;
when the central control module judges that the matching result meets a second preset condition, the central control module controls the arsine gas to be introduced into the pH value detector so as to detect the pH value of the arsine gas and compares the measured pH value PH of the arsine gas with parameters in a preset arsine gas pH value matrix PH 0:
if the PH is less than PH4, the central control module judges that the comparison result meets a third preset condition and further compares the PH with a matrix PH0, and if the PH is less than PH1, the central control module controls a first regulating valve to add an Mx1 amount of adsorbent; if the PH is not less than 1 and is less than 2, the central control module controls the first regulating valve to add the adsorbent with the amount of Mx 2; if the PH is not less than 2 and is less than 3, the central control module controls the first regulating valve to add the adsorbent with the amount of Mx 3; if the PH is not less than 3 and is less than 4, the central control module controls the first regulating valve to add the adsorbent with the amount of Mx 4;
and if the PH is greater than or equal to the PH4, the central control module judges that the comparison result does not meet a third preset condition.
According to the embodiment of the invention, the pH value of the arsine gas is compared with the parameters in the preset arsine gas pH value matrix PH0, and the amount of the added adsorbent is determined according to the comparison result, so that the acidic substances in the arsine gas can be reduced by controlling the first regulating valve to add the adsorbent, further, the impurities in the arsine gas can be effectively reduced, and the purity of the arsine is improved.
Specifically, the central control module is further provided with a preset sulfide content matrix S0 (S1, S2, S3, S4), wherein S1 represents a preset sulfide first content, S2 represents a preset sulfide second content, S3 represents a preset sulfide third content, and S4 represents a preset sulfide fourth content;
when the central control module judges that the comparison result does not meet a third preset condition, the central control module controls the arsine gas to be introduced into a sulfide detector to detect the sulfide content of the arsine gas and compares the detected sulfide content S with the parameters in a preset sulfide content matrix S0:
if S = Si, i =1,2,3,4, the central control module controls the first regulating valve to add Myi amounts of adsorbent, Myi = Mxi × η, where η represents an adsorbent adjustment coefficient and Mxi represents a value corresponding to a parameter in the preset adsorbent addition matrix Mx.
According to the embodiment of the invention, the content of the sulfide is compared with the parameters in the preset sulfide content matrix S0, and the amount of the added adsorbent is determined according to the comparison result, so that the first regulating valve is controlled to add the adsorbent to reduce the sulfide in the arsine gas, further, the impurities in the arsine gas can be effectively reduced, and the purity of the arsine is improved.
Specifically, the central control module is further provided with a preset carbon dioxide content difference interval matrix deltaC 0 (deltaC 1, deltaC 2, deltaC 3 and deltaC 4), wherein deltaC 1 represents a preset carbon dioxide content first difference interval, deltaC 2 represents a preset carbon dioxide content second difference interval, deltaC 3 represents a preset carbon dioxide content third difference interval, deltaC 4 represents a preset carbon dioxide content fourth difference interval, and the numerical ranges of the intervals are not overlapped;
the central control module is also provided with a preset molecular sieve specification matrix Q0(Q1, Q2, Q3 and Q4), wherein Q1 represents a molecular sieve with the specification of 3A, Q2 represents a molecular sieve with the specification of 4A, Q3 represents a molecular sieve with the specification of 5A, and Q4 represents a molecular sieve with the specification of 13A;
the central control module is also provided with a preset carbon dioxide content C0;
when the central control module judges that the comparison result does not meet a second preset condition, the central control module controls the arsine gas to be introduced into the carbon dioxide content detection device to detect the carbon dioxide content of the arsine gas and compares the detected carbon dioxide content C with a preset carbon dioxide content C0:
if C is less than or equal to C0, the central control module judges that the comparison result meets a fourth preset condition, which indicates that the content of carbon dioxide meets the standard;
if C is more than C0, the central control module judges that the comparison result does not meet a fourth preset condition and calculates the carbon dioxide content difference value delta C, delta C = C-C0, after the calculation is finished, the central control module matches the delta C with the parameters in a preset carbon dioxide content difference value interval matrix delta C0,
if the deltaC is in the deltaC 1 range, the central control module controls the second regulating valve to simultaneously select 1 molecular sieve with the specification of Q1 and 2 molecular sieves with the specification of Q2;
if the deltaC is in the deltaC 2 range, the central control module controls the second regulating valve to simultaneously select 2 molecular sieves with the specification of Q2 and 3 molecular sieves with the specification of Q3;
if the deltaC is in the deltaC 3 range, the central control module controls the second regulating valve to simultaneously select 3 molecular sieves with the specification of Q3 and 1 molecular sieve with the specification of Q4;
if the deltaC is in the deltaC 4 range, the central control module controls the second regulating valve to simultaneously select 3 molecular sieves with the specification of Q1 and 2 molecular sieves with the specification of Q4.
According to the embodiment of the invention, the specification of the molecular sieve selected by the second regulating valve is determined according to the comparison result by comparing the content of the carbon dioxide with the preset content of the carbon dioxide, so that the carbon dioxide in the arsine gas can be reduced by controlling the second regulating valve to select the molecular sieves with other specifications, further, the impurities in the arsine gas can be effectively reduced, and the purity of the arsine is improved.
Specifically, the central control module is further provided with a preset water vapor content matrix H0 (H1, H2, H3, H4), wherein H1 represents a first preset water vapor content, H2 represents a second preset water vapor content, H3 represents a third preset water vapor content, and H4 represents a fourth preset water vapor content;
when the central control module judges that the comparison result does not meet a second preset condition, the central control module controls the arsine gas to be introduced into the humidity meter so as to detect the water vapor content of the arsine gas and compares the detected water vapor content H with the parameters in a preset water vapor content matrix H0:
if H = Hi, i =1,2,3,4, the central control module controls the second regulating valve to select the molecular sieve with the Qi specification, where Qi represents the molecular sieve corresponding to the parameters in the preset molecular sieve specification matrix Q0.
According to the embodiment of the invention, the steam content is compared with the parameters in the preset steam content matrix H0, and the specification of the molecular sieve selected by the second regulating valve is determined according to the comparison result, so that the steam in the arsine gas can be reduced by controlling the second regulating valve to select the molecular sieves with other specifications, further, the impurities in the arsine gas can be effectively reduced, and the purity of the arsine is improved.
Specifically, the central control module is further provided with a preset molecular sieve selection coefficient matrix phi 0 (phi 1, phi 2, phi 3, phi 4), wherein phi 1 represents a first preset molecular sieve selection coefficient, phi 2 represents a second preset molecular sieve selection coefficient, phi 3 represents a third preset molecular sieve selection coefficient, and phi 4 represents a fourth preset molecular sieve selection coefficient;
the parameters in the preset water vapor content matrix H0 meet the conditions that H1 is more than H2 is more than H3 is more than H4;
when the central control module judges that the comparison result does not meet a fourth preset condition and selects the molecular sieve according to the matching relationship between the carbon dioxide content difference value and the parameters in the preset carbon dioxide content difference value interval matrix Delta C0, the central control module compares the measured water vapor content H with the parameters in the preset water vapor content matrix H0 and selects the molecular sieve according to the comparison result and the comparison result of the molecular sieve selection coefficient phi and the parameters in the preset molecular sieve selection coefficient matrix phi 0:
when H is less than H1, if phi = phi i, i =1,2,3,4, the central control module controls the second regulating valve to simultaneously select 1 molecular sieve with the specification of Q1 and 1 molecular sieve with the specification of Q2;
when H1 is not less than H < H2, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 2 molecular sieves with the specifications of Q2 and Q3;
when H2 is not less than H < H3, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 3 molecular sieves with the specifications of Q3 and Q4;
when H3 is not less than H < H4, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 4 molecular sieves with the specifications of Q1 and Q4;
when H is larger than or equal to H4, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 1Q 1, 2Q 2, 3Q 3 and 4Q 4 molecular sieves;
the calculation formula of the molecular sieve selection coefficient phi is as follows:
Φ=(H/Hi)/δ;
wherein, Hi represents the steam content corresponding to the parameters in the preset steam content matrix H0, δ represents the molecular sieve adjusting coefficient, i =1,2,3, 4.
According to the embodiment of the invention, the water vapor content is compared with the parameters in the preset water vapor content matrix, and the molecular sieve is selected according to the comparison result and the comparison result of the molecular sieve selection coefficient and the parameters in the preset molecular sieve selection coefficient matrix phi 0, so that the water vapor in the arsine gas can be reduced by controlling the second regulating valve to select the molecular sieves with other specifications, further, the impurities in the arsine gas can be effectively reduced, and the purity of the arsine is improved.
Specifically, the high-purity inert gas may be one of high-purity helium, neon, argon, or nitrogen.
Specifically, the molecular sieve is an activated alumina silica gel molecular sieve. The active alumina silica gel molecular sieve is formed by connecting at least one active alumina silica gel adsorption unit in series, can be repeatedly used and regenerated, has long service life and is more suitable for the requirements of users.
Specifically, the basic porous adsorbent comprises calcium oxide and sodium oxide. The calcium oxide and the sodium oxide are cheap and convenient to purchase, and the calcium oxide and the sodium oxide after impurity removal can be recycled after treatment, so that the overall performance of the whole device is greatly improved, and the requirements of users can be met.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for synthesizing and purifying arsine, which is characterized by comprising the following steps:
the method comprises the following steps: putting zinc powder and arsenic powder which are proportioned in advance into a quartz vessel, uniformly mixing, then putting into a stainless steel reaction tank after uniform mixing, vacuumizing, filling high-purity inert gas, and pressurizing and heating to obtain zinc arsenide powder for later use;
step two, putting the zinc arsenide powder collected in the step one into a reactor, and adding dilute sulfuric acid while stirring by using a stirrer to react to generate crude arsine gas;
step three, introducing the crude arsine gas obtained in the step two into an adsorption device, wherein an alkaline porous adsorbent and a molecular sieve are arranged in the adsorption device, so as to obtain arsine gas;
step four, trapping arsine gas in the step three by using a liquid nitrogen cold trap, condensing the arsine gas into liquid arsine, pumping out non-condensable gas by using a vacuum pump, taking down a liquid nitrogen tank outside the cold trap, and volatilizing the arsine to obtain pure arsine gas;
step five: introducing the arsine gas purified in the step five into a clean steel cylinder which is pretreated for storage to obtain a finished product;
the adsorption device and the liquid nitrogen tank are wirelessly connected with the central control module, the central control module is used for controlling the reaction process in the adsorption device, and a matrix is arranged in the central control module;
in the third step, the density of the arsine gas is periodically detected by using a density detector, the central control module calculates the comprehensive density of the arsine gas according to the density of the arsine gas periodically detected and compares the comprehensive density of the arsine gas with the preset comprehensive density of the arsine gas, and if the central control module judges that the comparison result meets a first preset condition, the next step is carried out; if the central control module judges that the comparison result does not accord with the first preset condition, the central control module calculates the arsine gas comprehensive density difference value and matches the arsine gas comprehensive density difference value with the parameters in a preset arsine gas comprehensive density difference value interval matrix delta rho 0, and if the central control module judges that the matching result accords with the second preset condition according to the matching result, the central control module controls a first regulating valve to add the adsorbent; if the central control module judges that the comparison result does not meet a second preset condition, the central control module controls a second regulating valve to select molecular sieves with other specifications;
the central control module establishes an arsine gas density matrix rho (rho 1, rho 2, rho 3, …, rho n) according to the arsine gas density periodically detected by the density monitor, wherein rho 1 represents the arsine gas density detected in the first detection period, rho 2 represents the arsine gas density detected in the second detection period, rho 3 represents the arsine gas density detected in the third detection period, and rho n represents the arsine gas density detected in the nth detection period, and is used for calculating the comprehensive density rhoz of the arsine gas, and the calculation formula is as follows:
ρz=(ρ1+ρ2+ρ3+…+ρn)/(n×α）；
wherein n represents n detection periods, and alpha represents an arsine gas density coefficient;
the central control module is provided with a preset arsine gas comprehensive density rho 0 for comparing with an arsine gas comprehensive density rho z:
if the rho z is not more than rho 0, the central control module tray bottom comparison result meets a first preset condition, and entering the next step;
and if the rho z is larger than the rho 0, the central control module judges that the comparison result does not meet a first preset condition.
2. The method of claim 1, wherein the central control module is further provided with a preset arsine gas integrated density difference interval matrix Δ ρ 0(Δ ρ 1, Δ ρ 2), wherein Δ ρ 1 represents a first difference interval of the preset arsine gas integrated density, and Δ ρ 2 represents a second difference interval of the preset arsine gas integrated density, and the numerical ranges of the intervals are not overlapped;
when the central control module judges that the comparison result does not meet a first preset condition, the central control module calculates the comprehensive density difference value delta rhoz of the arsine gas and matches the comprehensive density difference value delta rhoz with parameters in a preset comprehensive density difference value interval matrix delta rho 0 of the arsine gas:
if the delta rhoz is within the range of the delta rho 1, the central control module judges that the matching result meets a second preset condition and controls the first regulating valve to add the adsorbent;
if the delta rhoz is within the range of the delta rho 2, the central control module judges that the matching result does not meet a second preset condition and controls a second regulating valve to select molecular sieves with other specifications;
the calculation formula of the arsine gas comprehensive density difference delta rhoz is as follows:
△ρz=（ρz-ρ0）×β；
wherein beta represents the arsine gas integrated density difference coefficient.
3. The method of claim 2, wherein the central control module is further configured with a predetermined arsine gas PH value matrix PH0 (PH 1, PH2, PH3, PH 4), wherein PH1 represents a first predetermined arsine gas PH value, PH2 represents a second predetermined arsine gas PH value, PH3 represents a third predetermined arsine gas PH value, PH4 represents a fourth predetermined arsine gas PH value, PH1 < PH2 < PH3 < PH 4;
the central control module is further provided with a preset adsorbent adding matrix Mx (Mx1, Mx2, Mx3 and Mx4), wherein Mx1 represents a first adsorbent adding amount, Mx2 represents a second adsorbent adding amount, Mx3 represents a third adsorbent adding amount, and Mx4 represents a fourth adsorbent adding amount;
when the central control module judges that the matching result meets a second preset condition, the central control module controls the arsine gas to be introduced into the pH value detector so as to detect the pH value of the arsine gas and compares the measured pH value PH of the arsine gas with parameters in a preset arsine gas pH value matrix PH 0:
if the PH is less than PH4, the central control module judges that the comparison result meets a third preset condition and further compares the PH with a matrix PH0, and if the PH is less than PH1, the central control module controls a first regulating valve to add an Mx1 amount of adsorbent; if the PH is not less than 1 and is less than 2, the central control module controls the first regulating valve to add the adsorbent with the amount of Mx 2; if the PH is not less than 2 and is less than 3, the central control module controls the first regulating valve to add the adsorbent with the amount of Mx 3; if the PH is not less than 3 and is less than 4, the central control module controls the first regulating valve to add the adsorbent with the amount of Mx 4;
and if the PH is greater than or equal to the PH4, the central control module judges that the comparison result does not meet a third preset condition.
4. The method of claim 3, wherein the central control module is further configured with a predetermined sulfide content matrix S0 (S1, S2, S3, S4), wherein S1 represents a predetermined first sulfide content, S2 represents a predetermined second sulfide content, S3 represents a predetermined third sulfide content, and S4 represents a predetermined fourth sulfide content;
when the central control module judges that the comparison result does not meet a third preset condition, the central control module controls the arsine gas to be introduced into a sulfide detector to detect the sulfide content of the arsine gas and compares the detected sulfide content S with the parameters in a preset sulfide content matrix S0:
if S = Si, i =1,2,3,4, the central control module controls the first regulating valve to add Myi amounts of adsorbent, Myi = Mxi × η, where η represents an adsorbent adjustment coefficient and Mxi represents a value corresponding to a parameter in the preset adsorbent addition matrix Mx.
5. The method for synthesizing and purifying arsine of claim 1, wherein the central control module is further configured with a preset carbon dioxide content difference interval matrix ac 0 (ac 1, ac 2, ac 3, ac 4), wherein ac 1 represents a preset carbon dioxide content first difference interval, ac 2 represents a preset carbon dioxide content second difference interval, ac 3 represents a preset carbon dioxide content third difference interval, ac 4 represents a preset carbon dioxide content fourth difference interval, and the numerical ranges of the intervals are not overlapped;
the central control module is also provided with a preset molecular sieve specification matrix Q0(Q1, Q2, Q3 and Q4), wherein Q1 represents a molecular sieve with the specification of 3A, Q2 represents a molecular sieve with the specification of 4A, Q3 represents a molecular sieve with the specification of 5A, and Q4 represents a molecular sieve with the specification of 13A;
the central control module is also provided with a preset carbon dioxide content C0;
when the central control module judges that the comparison result does not meet a second preset condition, the central control module controls the arsine gas to be introduced into the carbon dioxide content detection device to detect the carbon dioxide content of the arsine gas and compares the detected carbon dioxide content C with a preset carbon dioxide content C0:
if C is less than or equal to C0, the central control module judges that the comparison result meets a fourth preset condition, which indicates that the content of carbon dioxide meets the standard;
if C is more than C0, the central control module judges that the comparison result does not meet a fourth preset condition and calculates the carbon dioxide content difference value delta C, delta C = C-C0, after the calculation is finished, the central control module matches the delta C with the parameters in a preset carbon dioxide content difference value interval matrix delta C0,
if the deltaC is in the deltaC 1 range, the central control module controls the second regulating valve to simultaneously select 1 molecular sieve with the specification of Q1 and 2 molecular sieves with the specification of Q2;
if the deltaC is in the deltaC 2 range, the central control module controls the second regulating valve to simultaneously select 2 molecular sieves with the specification of Q2 and 3 molecular sieves with the specification of Q3;
if the deltaC is in the deltaC 3 range, the central control module controls the second regulating valve to simultaneously select 3 molecular sieves with the specification of Q3 and 1 molecular sieve with the specification of Q4;
if the deltaC is in the deltaC 4 range, the central control module controls the second regulating valve to simultaneously select 3 molecular sieves with the specification of Q1 and 2 molecular sieves with the specification of Q4.
6. The method of claim 5, wherein the central control module is further configured with a predetermined steam content matrix H0 (H1, H2, H3, H4), wherein H1 represents a first predetermined steam content, H2 represents a second predetermined steam content, H3 represents a third predetermined steam content, and H4 represents a fourth predetermined steam content;
when the central control module judges that the comparison result does not meet a second preset condition, the central control module controls the arsine gas to be introduced into the humidity meter so as to detect the water vapor content of the arsine gas and compares the detected water vapor content H with the parameters in a preset water vapor content matrix H0:
if H = Hi, i =1,2,3,4, the central control module controls the second regulating valve to select the molecular sieve with the Qi specification, where Qi represents the molecular sieve corresponding to the parameters in the preset molecular sieve specification matrix Q0.
7. The method for synthesizing and purifying arsine of claim 5, wherein the central control module is further provided with a preset molecular sieve selection coefficient matrix Φ 0(Φ 1, Φ 2, Φ 3, Φ 4), wherein Φ 1 represents a preset molecular sieve first selection coefficient, Φ 2 represents a preset molecular sieve second selection coefficient, Φ 3 represents a preset molecular sieve third selection coefficient, and Φ 4 represents a preset molecular sieve fourth selection coefficient;
the parameters in the preset water vapor content matrix H0 meet the conditions that H1 is more than H2 is more than H3 is more than H4;
when the central control module judges that the comparison result does not meet a fourth preset condition and selects the molecular sieve according to the matching relationship between the carbon dioxide content difference value and the parameters in the preset carbon dioxide content difference value interval matrix Delta C0, the central control module compares the measured water vapor content H with the parameters in the preset water vapor content matrix H0 and selects the molecular sieve according to the comparison result and the comparison result of the molecular sieve selection coefficient phi and the parameters in the preset molecular sieve selection coefficient matrix phi 0:
when H is less than H1, if phi = phi i, i =1,2,3,4, the central control module controls the second regulating valve to simultaneously select 1 molecular sieve with the specification of Q1 and 1 molecular sieve with the specification of Q2;
when H1 is not less than H < H2, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 2 molecular sieves with the specifications of Q2 and Q3;
when H2 is not less than H < H3, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 3 molecular sieves with the specifications of Q3 and Q4;
when H3 is not less than H < H4, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 4 molecular sieves with the specifications of Q1 and Q4;
when H is larger than or equal to H4, if phi = phi i, the central control module controls the second regulating valve to simultaneously select 1Q 1, 2Q 2, 3Q 3 and 4Q 4 molecular sieves;
the calculation formula of the molecular sieve selection coefficient phi is as follows:
Φ=(H/Hi)/δ;
wherein, Hi represents the steam content corresponding to the parameters in the preset steam content matrix H0, δ represents the molecular sieve adjusting coefficient, i =1,2,3, 4.
8. The method of claim 1, wherein the high purity inert gas is one of high purity helium, neon, argon or nitrogen.
9. The method of claim 1, wherein the molecular sieve is an activated alumina silica molecular sieve.
10. The method of claim 1, wherein the basic porous adsorbent comprises calcium oxide and sodium oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011385329.6A CN112520699A (en) | 2020-12-01 | 2020-12-01 | Synthetic purification method of arsine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011385329.6A CN112520699A (en) | 2020-12-01 | 2020-12-01 | Synthetic purification method of arsine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112520699A true CN112520699A (en) | 2021-03-19 |
Family
ID=74995975
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011385329.6A Withdrawn CN112520699A (en) | 2020-12-01 | 2020-12-01 | Synthetic purification method of arsine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112520699A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115417452A (en) * | 2022-10-19 | 2022-12-02 | 铜仁学院 | Method for producing zinc arsenide by improved melt synthesis method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2203983C2 (en) * | 2001-03-13 | 2003-05-10 | Государственное унитарное предприятие "Государственный научно-исследовательский институт органической химии и технологии" | Process of electrochemical winning of hydrogen arsenide |
| JP2005008481A (en) * | 2003-06-19 | 2005-01-13 | Taiyo Toyo Sanso Co Ltd | Arsine purification method and apparatus |
| CN108414504A (en) * | 2018-03-16 | 2018-08-17 | 清远先导材料有限公司 | A method of measuring the reagent and a kind of special Gas content of measurement of special Gas content |
| CN110642227A (en) * | 2019-09-25 | 2020-01-03 | 博纯材料股份有限公司 | Synthetic purification method of arsine |
| CN110938830A (en) * | 2018-09-25 | 2020-03-31 | 东泰高科装备科技有限公司 | Safety control operation system of arsine gas preparation equipment |
-
2020
- 2020-12-01 CN CN202011385329.6A patent/CN112520699A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2203983C2 (en) * | 2001-03-13 | 2003-05-10 | Государственное унитарное предприятие "Государственный научно-исследовательский институт органической химии и технологии" | Process of electrochemical winning of hydrogen arsenide |
| JP2005008481A (en) * | 2003-06-19 | 2005-01-13 | Taiyo Toyo Sanso Co Ltd | Arsine purification method and apparatus |
| CN108414504A (en) * | 2018-03-16 | 2018-08-17 | 清远先导材料有限公司 | A method of measuring the reagent and a kind of special Gas content of measurement of special Gas content |
| CN110938830A (en) * | 2018-09-25 | 2020-03-31 | 东泰高科装备科技有限公司 | Safety control operation system of arsine gas preparation equipment |
| CN110642227A (en) * | 2019-09-25 | 2020-01-03 | 博纯材料股份有限公司 | Synthetic purification method of arsine |
Non-Patent Citations (1)
| Title |
|---|
| 胡玉亭: "高纯砷烷的合成", 《保定师范专科学校学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115417452A (en) * | 2022-10-19 | 2022-12-02 | 铜仁学院 | Method for producing zinc arsenide by improved melt synthesis method |
| CN115417452B (en) * | 2022-10-19 | 2024-05-14 | 铜仁学院 | Method for producing zinc arsenide by improved fusion synthesis method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5534172B2 (en) | Method for producing nitride crystal | |
| KR101095214B1 (en) | Divided electrochemical cell and low cost high purity hydride gas prodcution process | |
| CN102557035B (en) | Method for producing polycrystalline silicon rods | |
| US8940264B2 (en) | Process for producing polycrystalline silicon | |
| EP1977029A2 (en) | Crystalline composition, device, and associated method | |
| US20180371609A1 (en) | Method and system for preparing polycrystalline group iii metal nitride | |
| CN102502653A (en) | System and method for producing high-purity disilane | |
| CN112520699A (en) | Synthetic purification method of arsine | |
| CN110642227A (en) | Synthetic purification method of arsine | |
| CN112158847A (en) | Production and purification process of disilane | |
| US6712908B2 (en) | Purified silicon production system | |
| CN104925774B (en) | A kind of synthesis of electron level phosphine and purifying plant and method | |
| CN101857270A (en) | Method for synthesizing high-purity arsine | |
| CN1615271A (en) | Highly pure ultra-fine SiOx powder and method for production thereof | |
| KR20140082938A (en) | Cyclohexasilane and method of preparing the same | |
| US20090136409A1 (en) | Method for producing polycrystalline silicon | |
| CN102863023B (en) | Synthesis and purification method of electronic grade arsines | |
| WO2023226629A1 (en) | Deoxidizing and purifying method for mo source | |
| CN109721056A (en) | The method that depth removes impurity element in high-purity silicon carbide powder | |
| CN109133019A (en) | The development of high-purity phosphine scale continuous producing method and device | |
| CN111777039A (en) | Germane production process | |
| KR100800045B1 (en) | Method for preparing pure intermetallic compound of Ni3Al at low temperature | |
| JP2005187916A (en) | Solid high polymer type water electrolysis hydrogen production device | |
| JP2017160071A (en) | Ultrahigh purity mineralizer, and method of nitride crystal growth | |
| EP0245600A2 (en) | Process for the plasma synthesis of hydride compounds and apparatus for carrying out said process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20210319 |