CN105502295A - Electronic grade hydrogen chloride purification method - Google Patents
Electronic grade hydrogen chloride purification method Download PDFInfo
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- CN105502295A CN105502295A CN201511031134.0A CN201511031134A CN105502295A CN 105502295 A CN105502295 A CN 105502295A CN 201511031134 A CN201511031134 A CN 201511031134A CN 105502295 A CN105502295 A CN 105502295A
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- hydrogen chloride
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- reboiler
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
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Abstract
The invention provides an electronic grade hydrogen chloride purification method. The method is characterized by comprising the following steps: introducing industrial liquid hydrogen chloride with purity of 99% to the middle position of a first rectifying tower to be rectified so as to remove light components; introducing a liquid coming out from the bottom of a reboiler of the first rectifying tower to the middle position of a second rectifying tower by a pump to be rectified, condensing hydrogen chloride generated through heating by a second reboiler with a second condenser, controlling the reflux ratio, enabling part of hydrogen chloride to flow back to the second rectifying tower and transferring the other part of hydrogen chloride to middle storage tanks to be stored and pumping out residual liquid from the bottom of the second reboiler to a waste liquid storage tank so as to remove heavy components; and obtaining high-purity hydrogen chloride with purity above 99.9999% through adsorption and purification of at least an adsorption tower with a molecular sieve inside. The method has the effect of avoiding introduction of other impurity media, is simple to operate and is low in production cost.
Description
Technical field
The present invention relates to a kind of method of purification of electronic grade hydrogen chloride, belong to electronics special gas production purification field.
Background technology
Before electronic grade hydrogen chloride is mainly used in epitaxy, silicon and gallium arsenide high temperature gas phase etch, and remove sodium ion, high-purity hydrogen chloride is also for metallic surface chemical treatment in addition, and laser gas mixture, film are produced and surface treatment of carbon fibers.And high-purity hydrogen chloride is applied to medicine, chemical industry, semicon industry, therefore demand is increasing.The electronic grade hydrogen chloride product of China mostly from U.S., the import of Deng state, expensive.Therefore we need research further and the synthesis technique improving electronic grade hydrogen chloride, bring necessarily considerable social effect and economic benefit to China.
Existing research people successfully synthesizes electronic grade hydrogen chloride in research preparation process at present, from these synthetic methods, find method of analysis and hydrochloric acid is de-analyses legal system and simply can be mass-produced for hydrogenchloride technique simultaneously, but the hydrogenchloride purity of preparation is on the low side, more and more do not meet electronic industry, especially the requirement of unicircuit.The purity that synthesis method produces hydrogenchloride is higher, but wherein the water yield is high, seriously corroded, and high to equipment requirements, production cost is high.Consider the many factors such as environmental protection, preparation high purity hydrogenchloride is inevitable development trend.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of electronic grade hydrogen chloride method of purification, with low cost, production safety and can realize continuous print scale operation.
In order to solve the problems of the technologies described above, the invention provides a kind of method of purification of electronic grade hydrogen chloride, it is characterized in that, comprising:
The first step: by the purity of technical grade be 99% the liquid hydrogenchloride mid-way that is incorporated into the first rectifying tower carry out rectifying, the tower top of the first rectifying tower connects the first condenser, the first reboiler is connected at the bottom of tower, thermogenetic hydrogen chloride gas is added after the first condenser condenses in total reflux to the first rectifying tower through the first reboiler, uncooled waste gas enters to flare system, to remove light constituent;
Second step: rectifying is carried out in the mid-way that liquid pump is out incorporated into Second distillation column bottom the first rectifying tower reboiler, the tower top of Second distillation column connects the second condenser, the second reboiler is connected at the bottom of tower, thermogenetic hydrogen chloride gas is added through the second condenser condenses through the second reboiler, control reflux ratio, make it be partly refluxed in Second distillation column, another part proceeds in relay tank and stores, bottom the second reboiler, raffinate is drawn to waste tank, to remove heavy constituent;
3rd step: the liquid hydrogenchloride in relay tank is heated, add thermogenetic hydrogen chloride gas is provided with molecular sieve absorption tower adsorbs purifying through at least one inside, the purity obtained is the high-purity hydrogen chloride of more than 99.9999%, adopts the finished product storage tank being placed in liquid nitrogen cold trap to collect.
Preferably, the first described rectifying tower is packing tower, and its theoretical plate number is 12 ~ 24, and rectifying pressure is at 10 ~ 15bar, and tower top temperature is-20 ~-30 DEG C, and column bottom temperature is-10 ~ 10 DEG C.
Preferably, described Second distillation column is packing tower, and its theoretical plate number is 12 ~ 24, and rectifying pressure is at 10 ~ 15bar, and tower top temperature is-20 ~-30 DEG C, and column bottom temperature is-10 ~ 10 DEG C.
More preferably, the first described rectifying tower and Second distillation column filler used are Hastelloy material.
Preferably, the reflux ratio in described second step is between 1.5 ~ 2.5.
Preferably, the adsorption tower in the 3rd described step has at least one, mutually connects.
Preferably, the aluminum oxide molecular sieve of described molecular sieve to be specification be 3A, 4A or 5A.
Preferably, the first described rectifying tower, the first reboiler, Second distillation column, the second reboiler, relay tank and finished product storage tank all adopt Hastelloy material.
Preferably, the 3rd described step is heated to 30 ~ 45 DEG C.
Compared with prior art, the invention has the beneficial effects as follows:
The method of purification of electronic grade hydrogen chloride of the present invention directly adopts the liquid hydrogenchloride of common technical grade to carry out secondary low temperature fractionation, and then adsorbed by molecular sieve, after secondary rectifying, the purity of finished product can management and control and guarantee well, the raffinate that rectifying produces can also be sold as lower technical grade substandard goods, the molecular sieve of absorption can reuse, and significantly reduces production cost.Method of purification of the present invention, without the need to additional reaction medium, thus avoids the introducing of other impurity medium, and simple to operate, and production cost is low.
Accompanying drawing explanation
Fig. 1 is the purifying plant schematic diagram of electronic grade hydrogen chloride.In figure, 1 is raw material steel cylinder, and 2 is the first rectifying tower, and 3 is the first condenser, and 4 is the first reboiler, and 5 is pump, and 6 is Second distillation column, and 7 is the second condenser, and 8 is the second reboiler, and 9 is relay tank, and 10 is adsorption tower, and 11 is finished product storage tank.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.Each equipment in the purifying plant used in various embodiments of the present invention is commercially available prod.Described the first rectifying tower 2, first reboiler 4, Second distillation column 6, second reboiler 8, relay tank 9 and finished product storage tank 11 all adopt Hastelloy material.
Embodiment 1
As shown in Figure 1, the method for purification concrete steps of the electronic grade hydrogen chloride of the present embodiment are:
The first step: by the purity of technical grade be 99% the liquid hydrogenchloride mid-way that is incorporated into the first rectifying tower 2 carry out rectifying, the first described rectifying tower 2 is packing tower, filler used is the Raschig ring shape filler of Hastelloy material, its theoretical plate number is 24, rectifying pressure is at 10bar, tower top temperature is-20 DEG C, column bottom temperature is 10 DEG C, the tower top of the first rectifying tower connects the first condenser 3, the first reboiler 4 is connected at the bottom of tower, first reboiler 4 uses electric heating blanket to heat, thermogenetic hydrogen chloride gas is added after the first condenser 3 condensation in total reflux to the first rectifying tower 2 through the first reboiler 4, uncooled waste gas enters to flare system, to remove light constituent as nitrogen, oxygen, hydrogen, carbon monoxide etc.,
Second step: rectifying is carried out in the mid-way that liquid pump is out incorporated into Second distillation column 6 bottom the first rectifying tower reboiler, described Second distillation column 6 is packing tower, filler used is the Raschig ring shape filler of Hastelloy material, its theoretical plate number is 24, rectifying pressure is at 10bar, tower top temperature is-20 DEG C, column bottom temperature is 10 DEG C, the tower top of Second distillation column 6 connects the second condenser 7, the second reboiler 8 is connected at the bottom of tower, second reboiler 8 uses electric heating blanket to heat, thermogenetic hydrogen chloride gas is added through the second condenser 7 condensation through the second reboiler 8, controlling reflux ratio is 1.5, it is made to be partly refluxed in Second distillation column 6, another part proceeds in relay tank 9 and stores, bottom the second reboiler 8, raffinate pump is drawn to waste tank, to remove heavy constituent as moisture etc., tower bottoms can be used as industrial raw material and separately uses it for anything else,
3rd step: use electric heating blanket to be heated to 30 DEG C to the liquid hydrogenchloride in relay tank 9, add thermogenetic hydrogen chloride gas is provided with 3A aluminum oxide molecular sieve adsorption tower 10 adsorption and purification through the inside of three series connection, the impurity such as further removing moisture and carbonic acid gas, obtain high-purity hydrogen chloride, adopt the finished product storage tank 11 being placed in liquid nitrogen cold trap to collect.Adopt the analytical instrument such as gas-chromatography, Moisture Meter to analyze finished product high-purity hydrogen chloride, the purity of analytical results display electronic grade hydrogen chloride is more than 99.9999%.
Embodiment 2
As shown in Figure 1, the method for purification concrete steps of the electronic grade hydrogen chloride of the present embodiment are:
The first step: by the purity of technical grade be 99% the liquid hydrogenchloride mid-way that is incorporated into the first rectifying tower 2 carry out rectifying, the first described rectifying tower 2 is packing tower, filler used is the Bauer ring packing of Hastelloy material, its theoretical plate number is 20, rectifying pressure is at 12bar, tower top temperature is-25 DEG C, column bottom temperature is 0 DEG C, the tower top of the first rectifying tower connects the first condenser 3, the first reboiler 4 is connected at the bottom of tower, first reboiler 4 uses heat-conducting oil heating, thermogenetic hydrogen chloride gas is added after the first condenser 3 condensation in total reflux to the first rectifying tower 2 through the first reboiler 4, uncooled waste gas enters to flare system, to remove light constituent as nitrogen, oxygen, hydrogen, carbon monoxide etc.,
Second step: rectifying is carried out in the mid-way that liquid pump is out incorporated into Second distillation column 6 bottom the first rectifying tower reboiler, described Second distillation column 6 is packing tower, filler used is the Bauer ring packing of Hastelloy material, its theoretical plate number is 20, rectifying pressure is at 12bar, tower top temperature is-25 DEG C, column bottom temperature is 0 DEG C, the tower top of Second distillation column 6 connects the second condenser 7, the second reboiler 8 is connected at the bottom of tower, second reboiler 8 uses thermal oil coil pipe to heat, thermogenetic hydrogen chloride gas is added through the second condenser 7 condensation through the second reboiler 8, controlling reflux ratio is 2, it is made to be partly refluxed in Second distillation column 6, another part proceeds in relay tank 9 and stores, bottom the second reboiler 8, raffinate pump is drawn to waste tank, to remove heavy constituent as moisture etc.,
3rd step: use thermal oil to be heated to 35 DEG C to the liquid hydrogenchloride in relay tank 9, add thermogenetic hydrogen chloride gas is provided with 4A aluminum oxide molecular sieve adsorption tower 10 adsorption and purification through the inside of three series connection, the impurity such as further removing moisture and carbonic acid gas, obtain high-purity hydrogen chloride, adopt the finished product storage tank 11 being placed in liquid nitrogen cold trap to collect.Adopt the analytical instrument such as gas-chromatography, Moisture Meter to analyze finished product high-purity hydrogen chloride, the purity of analytical results display electronic grade hydrogen chloride is more than 99.9999%.
Embodiment 3
As shown in Figure 1, the method for purification concrete steps of the electronic grade hydrogen chloride of the present embodiment are:
The first step: by the purity of technical grade be 99% the liquid hydrogenchloride mid-way that is incorporated into the first rectifying tower 2 carry out rectifying, the first described rectifying tower 2 is packing tower, filler used is the cascade ring packing of Hastelloy material, its theoretical plate number is 12, rectifying pressure is at 15bar, tower top temperature is-30 DEG C, column bottom temperature is-10 DEG C, the tower top of the first rectifying tower connects the first condenser 3, the first reboiler 4 is connected at the bottom of tower, first reboiler 4 uses electric heating blanket to heat, thermogenetic hydrogen chloride gas is added after the first condenser 3 condensation in total reflux to the first rectifying tower 2 through the first reboiler 4, uncooled waste gas enters to flare system, to remove light constituent as nitrogen, oxygen, hydrogen, carbon monoxide etc.,
Second step: rectifying is carried out in the mid-way that liquid pump is out incorporated into Second distillation column 6 bottom the first rectifying tower reboiler, described Second distillation column 6 is packing tower, filler used is the cascade ring packing of Hastelloy material, its theoretical plate number is 12, rectifying pressure is at 15bar, tower top temperature is-30 DEG C, column bottom temperature is-10 DEG C, the tower top of Second distillation column 6 connects the second condenser 7, the second reboiler 8 is connected at the bottom of tower, second reboiler 8 uses electric heating blanket to heat, thermogenetic hydrogen chloride gas is added through the second condenser 7 condensation through the second reboiler 8, controlling reflux ratio is 2.5, it is made to be partly refluxed in Second distillation column 6, another part proceeds in relay tank 9 and stores, bottom the second reboiler 8, raffinate pump is drawn to waste tank, to remove heavy constituent as moisture etc.,
3rd step: use electric heating blanket to be heated to 40 DEG C to the liquid hydrogenchloride in relay tank 9, add thermogenetic hydrogen chloride gas is provided with 5A aluminum oxide molecular sieve adsorption tower 10 adsorption and purification through the inside of three series connection, the impurity such as further removing moisture and carbonic acid gas, obtain high-purity hydrogen chloride, adopt the finished product storage tank 11 being placed in liquid nitrogen cold trap to collect.Adopt the analytical instrument such as gas-chromatography, Moisture Meter to analyze finished product high-purity hydrogen chloride, the purity of analytical results display electronic grade hydrogen chloride is more than 99.9999%.
Claims (9)
1. a method of purification for electronic grade hydrogen chloride, is characterized in that, comprising:
The first step: by the purity of technical grade be 99% the liquid hydrogenchloride mid-way that is incorporated into the first rectifying tower (2) carry out rectifying, the tower top of the first rectifying tower connects the first condenser (3), the first reboiler (4) is connected at the bottom of tower, thermogenetic hydrogen chloride gas is added after the first condenser (3) condensation in total reflux to the first rectifying tower (2) through the first reboiler (4), uncooled waste gas enters to flare system, to remove light constituent;
Second step: rectifying is carried out in the mid-way that liquid pump is out incorporated into Second distillation column (6) bottom the first rectifying tower reboiler, the tower top of Second distillation column (6) connects the second condenser (7), the second reboiler (8) is connected at the bottom of tower, thermogenetic hydrogen chloride gas is added through the second condenser (7) condensation through the second reboiler (8), control reflux ratio, it is made to be partly refluxed in Second distillation column (6), another part proceeds in relay tank (9) and stores, from the second reboiler (8) bottom, raffinate is drawn to waste tank, to remove heavy constituent,
3rd step: the liquid hydrogenchloride in relay tank (9) is heated, add thermogenetic hydrogen chloride gas is provided with molecular sieve adsorption tower (10) adsorption and purification through at least one inside, the purity obtained is the high-purity hydrogen chloride of more than 99.9999%, adopts the finished product storage tank (11) being placed in liquid nitrogen cold trap to collect.
2. the method for purification of electronic grade hydrogen chloride as claimed in claim 1, it is characterized in that, described the first rectifying tower (2) is packing tower, its theoretical plate number is 12 ~ 24, rectifying pressure is at 10 ~ 15bar, and tower top temperature is-20 ~-30 DEG C, and column bottom temperature is-10 ~ 10 DEG C.
3. the method for purification of electronic grade hydrogen chloride as claimed in claim 1, it is characterized in that, described Second distillation column (6) is packing tower, its theoretical plate number is 12 ~ 24, rectifying pressure is at 10 ~ 15bar, and tower top temperature is-20 ~-30 DEG C, and column bottom temperature is-10 ~ 10 DEG C.
4. the method for purification of electronic grade hydrogen chloride as claimed in claim 3, is characterized in that, described the first rectifying tower (2) and Second distillation column (6) filler used are Hastelloy material.
5. the method for purification of electronic grade hydrogen chloride as claimed in claim 1, it is characterized in that, the reflux ratio in described second step is between 1.5 ~ 2.5.
6. the method for purification of electronic grade hydrogen chloride as claimed in claim 1, it is characterized in that, the adsorption tower (10) in the 3rd described step has at least one, mutually connects.
7. the method for purification of electronic grade hydrogen chloride as claimed in claim 1, is characterized in that, the aluminum oxide molecular sieve of described molecular sieve to be specification be 3A, 4A or 5A.
8. the method for purification of electronic grade hydrogen chloride as claimed in claim 1, it is characterized in that, described the first rectifying tower (2), the first reboiler (4), Second distillation column (6), the second reboiler (8), relay tank (9) and finished product storage tank (11) all adopt Hastelloy material.
9. the method for purification of electronic grade hydrogen chloride as claimed in claim 1, it is characterized in that, the 3rd described step is heated to 30 ~ 40 DEG C.
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Cited By (12)
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CN106044710A (en) * | 2016-07-19 | 2016-10-26 | 浙江博瑞电子科技有限公司 | Method for purifying electron-grade hydrogen chloride |
CN106276796A (en) * | 2016-07-19 | 2017-01-04 | 浙江博瑞电子科技有限公司 | A kind of method preparing high-purity hydrogen chloride |
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CN110980648A (en) * | 2019-12-31 | 2020-04-10 | 中船重工(邯郸)派瑞特种气体有限公司 | Hydrogen bromide purification device and method |
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CN106044710B (en) * | 2016-07-19 | 2019-07-12 | 浙江博瑞电子科技有限公司 | A kind of method of purification of electronic grade hydrogen chloride |
CN106044710A (en) * | 2016-07-19 | 2016-10-26 | 浙江博瑞电子科技有限公司 | Method for purifying electron-grade hydrogen chloride |
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CN109650340A (en) * | 2018-12-26 | 2019-04-19 | 江阴江化微电子材料股份有限公司 | A kind of method for producing electronic grade hydrochloric acid |
CN110255501A (en) * | 2019-07-11 | 2019-09-20 | 金宏气体电子材料(淮安)有限责任公司 | A kind of electronic grade high-purity hydrogen chloride preparation method |
CN110526213A (en) * | 2019-10-14 | 2019-12-03 | 苏州金宏气体股份有限公司 | A kind of hydrogen bromide purification process |
CN110980648A (en) * | 2019-12-31 | 2020-04-10 | 中船重工(邯郸)派瑞特种气体有限公司 | Hydrogen bromide purification device and method |
CN111115579A (en) * | 2020-01-12 | 2020-05-08 | 浙江博瑞电子科技有限公司 | Reactive ultrasonic rectification purification method for HCL electronic gas |
CN111115579B (en) * | 2020-01-12 | 2021-12-17 | 浙江博瑞电子科技有限公司 | Reactive ultrasonic rectification purification method for HCL electronic gas |
CN112546659A (en) * | 2020-12-08 | 2021-03-26 | 云南临沧鑫圆锗业股份有限公司 | Purification device and method for germanium tetrafluoride |
CN112546659B (en) * | 2020-12-08 | 2022-02-15 | 云南临沧鑫圆锗业股份有限公司 | Purification device and method for germanium tetrafluoride |
CN114082211A (en) * | 2021-10-31 | 2022-02-25 | 中船(邯郸)派瑞特种气体股份有限公司 | Device for producing electronic grade hydrogen chloride based on partition plate tower |
CN114082211B (en) * | 2021-10-31 | 2023-09-22 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for producing electronic grade hydrogen chloride based on baffle tower |
CN114195098A (en) * | 2022-01-06 | 2022-03-18 | 新地能源工程技术有限公司 | Electronic grade hydrogen bromide preparation device and process |
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