CN117398707A - Electronic grade hexamethyldisilazane purification device and purification method - Google Patents
Electronic grade hexamethyldisilazane purification device and purification method Download PDFInfo
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- CN117398707A CN117398707A CN202311151895.4A CN202311151895A CN117398707A CN 117398707 A CN117398707 A CN 117398707A CN 202311151895 A CN202311151895 A CN 202311151895A CN 117398707 A CN117398707 A CN 117398707A
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- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 title claims abstract description 170
- 238000000746 purification Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000001179 sorption measurement Methods 0.000 claims abstract description 45
- 238000003860 storage Methods 0.000 claims abstract description 41
- 239000011347 resin Substances 0.000 claims abstract description 32
- 229920005989 resin Polymers 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 239000002699 waste material Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 27
- 239000012535 impurity Substances 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000741 silica gel Substances 0.000 claims description 18
- 229910002027 silica gel Inorganic materials 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- 238000005070 sampling Methods 0.000 claims description 17
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 150000001768 cations Chemical class 0.000 claims description 8
- 239000003729 cation exchange resin Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000003463 adsorbent Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000002912 waste gas Substances 0.000 claims description 3
- 238000011033 desalting Methods 0.000 claims description 2
- 239000003456 ion exchange resin Substances 0.000 claims description 2
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 239000000047 product Substances 0.000 description 44
- 229910021645 metal ion Inorganic materials 0.000 description 9
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 6
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 description 5
- 238000005342 ion exchange Methods 0.000 description 4
- 229920002120 photoresistant polymer Polymers 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000010612 desalination reaction Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 aerospace Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/10—Compounds having one or more C—Si linkages containing nitrogen having a Si-N linkage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
- B01D15/361—Ion-exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses an electronic-grade hexamethyldisilazane purification device and a purification method, wherein the electronic-grade hexamethyldisilazane purification device comprises a raw material storage tank, a discharge port of the raw material storage tank is connected with a feed end of a light-removal rectifying tower through a pipeline, a discharge port at the bottom of the light-removal rectifying tower is connected with a feed port of a heavy-removal rectifying tower through a pipeline, an air outlet at the top of the light-removal rectifying tower is connected with a first condenser inlet through a pipeline, a first condenser outlet is connected with a waste storage tank through a pipeline, an air outlet at the top of the heavy-removal rectifying tower is connected with a second condenser inlet through a pipeline, a second condenser outlet is connected with a feed port of the rectifying storage tank through a pipeline, a discharge port of the rectifying storage tank is connected with a feed port of a resin adsorption system through a pipeline, and a discharge port of the resin adsorption system is connected with a feed port of a product tank through a pipeline; the invention greatly improves the purity of the product and meets the quality requirement of semiconductors.
Description
Technical Field
The invention relates to the technical field of preparation of ultrahigh-purity process chemicals used in semiconductor manufacturing, in particular to an electronic-grade hexamethyldisilazane purification device and a purification method.
Background
Hexamethyldisilazane is an important organosilicon material and has wide application in the fields of medicine, aerospace, semiconductor manufacturing and the like. In the electronic industry, ultra-clean high purity reagents are extremely harsh on impurity content and granularity in the preparation process, and are widely applied to the field of integrated circuits. Adhesion is poor due to the difference in hydrophilicity and hydrophobicity of the photoresist and wafer. Localized gaps or bubbles may be caused when photoresist is applied, and the thickness and uniformity of the applied photoresist may be affected. And hexamethyldisilazane is introduced as a surfactant, so that the adhesiveness of the photoresist and the substrate can be improved, and the lateral etching of the etching liquid entering the mask and the substrate can be effectively inhibited.
The hexamethyldisilazane is hydrolyzed to generate hexamethyldisiloxane and trimethylsilanol, and the hexamethyldisiloxane and the trimethylsilanol are usually mixed together when the hexamethyldisilazane is prepared, and the hexamethyldisiloxane and the trimethylsilanol are required to be separated and purified by rectification, but the purity of the product is not high due to the fact that only part of moisture, metal ions and particles can be removed by rectification, the quality of the product is seriously influenced, and the quality requirement of a semiconductor is not met.
Disclosure of Invention
The invention aims to overcome the defects and provide an electronic-grade hexamethyldisilazane purifying device and a purifying method, so that the purity of a product is improved and the quality requirement of a semiconductor is met.
The invention aims to solve the technical problems, and adopts the technical scheme that: the utility model provides an electronic grade hexamethyldisilazane purification device, includes the raw materials storage tank, the raw materials storage tank discharge gate passes through the pipeline and is connected with the dealcoholization rectifying column feed end, and dealcoholization rectifying column bottom discharge gate passes through the pipeline and is connected with the dealcoholization rectifying column feed inlet, and the dealcoholization rectifying column top gas outlet passes through pipeline and first condenser access connection, and first condenser export passes through the pipeline and is connected with the waste material storage tank, the dealcoholization rectifying column top gas outlet passes through pipeline and second condenser access connection, and the second condenser export passes through the pipeline and is connected with rectifying tank feed inlet, rectifying tank discharge gate passes through the pipeline and is connected with resin adsorption system feed inlet, and resin adsorption system discharge gate passes through the pipeline and is connected with filtration system feed inlet, and filtration system discharge gate passes through the pipeline and is connected with product tank feed inlet.
Preferably, the extraction opening at the top of the product tank is connected with one end of the vacuum tank through a pipeline, and the other end of the vacuum tank is connected with the vacuum pump through a pipeline.
Preferably, the discharge hole at the bottom of the product tank is connected with one end of the product pump through a pipeline, and the other end of the product pump is connected with the sampling box through a pipeline.
Preferably, the pipeline where the feed inlet of the product tank is located is provided with a first valve, the pipeline where the extraction opening at the top of the product tank is located is provided with a second valve, and the pipeline where the discharge outlet at the bottom of the product tank is located is provided with a third valve.
Preferably, a silica gel adsorption system is arranged on a pipeline where the feed inlet of the raw material storage tank is located, and a first feed pump is arranged on a pipeline between the discharge outlet of the raw material storage tank and the feed inlet of the light component removal rectifying tower.
Preferably, a second feed pump is arranged on a pipeline between the discharge port of the rectifying storage tank and the feed port of the resin adsorption system.
Preferably, the adsorbent adopted by the resin adsorption system is cation exchange resin, and the filter element adopted by the filter system has the filter precision of 0.02 mu m.
In addition, the invention also discloses a purification method of the electronic grade hexamethyldisilazane purification device, which comprises the following steps:
s1: raw materials enter a silica gel adsorption system through a pipeline, are subjected to silica gel adsorption treatment to remove part of water, and are pumped into a raw material storage tank;
s2: materials in the raw material storage tank sequentially pass through a light-removal rectifying tower and a heavy-removal rectifying tower to carry out a rectifying process, light components-trimethylsilanol and hexamethyldisiloxane in the industrial-grade hexamethyldisilazane are separated through the light-removal rectifying tower, and heavy components-metal impurities and partial particles in the industrial-grade hexamethyldisilazane are separated through the heavy-removal rectifying tower; then the materials are sent into a rectification storage tank;
s3: the material in the rectifying storage tank passes through a resin adsorption system, and cation in hexamethyldisilazane is subjected to ion exchange by utilizing ion exchange resin, so that the cation in the material is transferred to the resin, and the aim of desalting is fulfilled;
s4: the materials treated by the resin adsorption system enter a filtering system, and solid particles in hexamethyldisilazane are trapped on the materials, so that the operation of solid-liquid separation is realized; removing particles in hexamethyldisilazane to obtain electronic-grade hexamethyldisilazane, and delivering the electronic-grade hexamethyldisilazane into a product tank.
Further, the step S4 further includes the following steps:
s4.1, before the electronic-grade hexamethyldisilazane is sent into a product tank, a first valve of a pipeline where a feed inlet of the product tank is positioned is closed, a third valve of a pipeline where a discharge outlet of the bottom of the product tank is positioned, a second valve of a pipeline where an extraction opening of the top of the product tank is positioned is opened, and a vacuum pump works to generate negative pressure, so that the product tank and a sampling tank are kept in a vacuum state, waste gas in the product tank and the sampling tank is sucked into the vacuum tank, and then the second valve and the third valve are closed;
s4.2, opening a first valve, and enabling materials to enter a product tank;
s4.3, when sampling is needed, opening a third valve, and allowing materials to enter the sampling box from the product tank.
The invention has the beneficial effects that: the invention separates light components-trimethyl silanol and hexamethyldisilazane in the industrial grade hexamethyldisilazane by the light component removal rectifying tower, separates heavy components-metal impurities and partial particles in the industrial grade hexamethyldisilazane by the heavy component removal rectifying tower, and the metal ions and partial particles impurities in the rectified hexamethyldisilazane can be further removed by the resin adsorption system and the filtering system, the content of the hexamethyldisilazane reaches more than 99.99 percent, the purity of the product is greatly improved, and the quality requirement of semiconductors is met.
Drawings
FIG. 1 is a schematic diagram of an electronic grade hexamethyldisilazane purification apparatus and purification method.
Detailed Description
The invention is described in further detail below with reference to the drawings and the specific examples.
As shown in figure 1, an electronic grade hexamethyldisilazane purification device comprises a raw material storage tank 1, a discharge port of the raw material storage tank 1 is connected with a feed end of a light-removal rectifying tower 4 through a pipeline, a discharge port at the bottom of the light-removal rectifying tower 4 is connected with a feed port of a heavy-removal rectifying tower 7 through a pipeline, an air outlet at the top of the light-removal rectifying tower 4 is connected with a first condenser 5 through a pipeline, an air outlet at the top of the light-removal rectifying tower 5 is connected with a waste storage tank 6 through a pipeline, an air outlet at the top of the heavy-removal rectifying tower 7 is connected with a second condenser 8 through a pipeline, an outlet of the second condenser 8 is connected with a feed port of a rectifying storage tank 9 through a pipeline, a discharge port of the rectifying storage tank 9 is connected with a feed port of a resin adsorption system 11 through a pipeline, a discharge port of the resin adsorption system 11 is connected with a feed port of a filtering system 12 through a pipeline, and a discharge port of the filtering system 12 is connected with a feed port of a product tank 13 through a pipeline.
Preferably, the top air extraction opening of the product tank 13 is connected with one end of the vacuum tank 16 through a pipeline, and the other end of the vacuum tank 16 is connected with the vacuum pump 17 through a pipeline.
Preferably, a discharge hole at the bottom of the product tank 13 is connected with one end of the product pump 14 through a pipeline, and the other end of the product pump 14 is connected with the sampling box 15 through a pipeline.
Preferably, the pipeline at the feed inlet of the product tank 13 is provided with a first valve 18, the pipeline at the extraction opening at the top of the product tank 13 is provided with a second valve 19, and the pipeline at the discharge outlet at the bottom of the product tank 13 is provided with a third valve 20.
Preferably, a silica gel adsorption system 2 is arranged on a pipeline where a feed inlet of the raw material storage tank 1 is located, and a first feed pump 3 is arranged on a pipeline between a discharge outlet of the raw material storage tank 1 and a feed inlet of the light component removal rectifying tower 4. The silica gel adsorbent in the silica gel adsorption system 2 needs to be dehydrated before being used, is heated to 100-110 ℃, and is kept for 5 hours, so that the moisture adsorbed by hydrogen bonds on the surface of the silica gel adsorbent is removed.
Preferably, a second feed pump 10 is arranged on a pipeline between the discharge port of the rectifying tank 9 and the feed port of the resin adsorption system 11.
Preferably, the adsorbent used in the resin adsorption system 11 is cation exchange resin, and the filter element selected in the filter system 12 has a filter accuracy of 0.02 μm. In this example, the cation exchange resin was selected from the group consisting of model UP 6150. The filtering system is composed of a PP framework, a PTFE membrane and a PFA filter shell. Before using, the cation exchange resin needs to be activated, soaked by ethanol, washed to be strong acid by 5% hydrochloric acid, washed to be neutral by distilled water, washed to be strong alkaline by 5% sodium hydroxide, then washed to be neutral by water, washed for three times by acid-water-alkali-water, then washed to be strong acid, and washed to be neutral by distilled water, thus the cation exchange resin can be used.
In the above technical solution, the light component removing rectifying tower 4 and heavy component removing rectifying tower 7 are plate type towers or packed towers, preferably packed towers. When the rectifying column is a packed column, the packing may be a metal or nonmetal structured or a bulk packing, preferably a bulk packing.
In addition, the invention also discloses a purification method of the electronic grade hexamethyldisilazane purification device, which comprises the following steps:
s1: raw materials enter a silica gel adsorption system 2 through a pipeline, are subjected to silica gel adsorption treatment to remove part of water, and are pumped into a raw material storage tank 1; in the step, through the affinity between the hydroxyl on the surface of the silica gel and water molecules in hexamethyldisilazane, water absorption is realized, and the silica gel is conveyed into a raw material storage tank, so that the stable quality of a product can be ensured, the fluctuation of a system is reduced, and the influence of the fluctuation of the raw material on the quality of the product can be reduced, and meanwhile, the quality of the product is further improved.
S2: the materials in the raw material storage tank 1 sequentially pass through a light removal rectifying tower 4 and a heavy removal rectifying tower 7 for rectification, light components-trimethylsilanol and hexamethyldisiloxane in the industrial-grade hexamethyldisilazane are separated by the light removal rectifying tower 4, and heavy components-metal impurities and partial particles in the industrial-grade hexamethyldisilazane are separated by the heavy removal rectifying tower 7; in the process, light component impurities enter a first condenser 5 through an air outlet at the top of a light component removal rectifying tower 4, and enter a waste storage tank 6 after being condensed; and heavy component impurities remain at the bottom of the heavy component removal rectifying tower 7; the light component materials in the de-heavy rectifying tower 7 enter a second condenser 8 through a top air outlet, and enter a rectifying storage tank 9 after being condensed; in the step, the temperature of the top of the rectifying tower for rectifying treatment is 30-40 ℃. In the step, the light components in the industrial-grade hexamethyldisilazane, including trimethylsilanol, hexamethyldisilazane and the like, are separated by utilizing the light component removal rectifying tower 4, and the remaining components are sent into the heavy component removal rectifying tower 7 to remove the components, such as metal impurities, particulate matters and the like, so as to obtain the hexamethyldisilazane with higher purity.
S3: the material in the rectifying storage tank 9 passes through a resin adsorption system 11, and cation in hexamethyldisilazane is fed into the resin adsorption system by utilizing ion exchange resinPerforming ion exchange to transfer cations in the material to resin, so as to achieve the aim of desalination; in this step, H on the cation exchange resin is passed through + Ion exchange with the cation in hexamethyldisilazane, so that the cation in solution is transferred to the resin, and H on the resin + Exchange into the solution, thereby achieving the purpose of desalination.
S4: the material treated by the resin adsorption system 11 enters the filtering system 12, and solid particles in hexamethyldisilazane are trapped on the material, so that the operation of solid-liquid separation is realized; after removal of the particulate matter from hexamethyldisilazane, electronic grade hexamethyldisilazane is obtained and fed into the product tank 13. In this step, hexamethyldisilazane is passed through the pore canal of the porous medium in the filtration system 12 by external force, and the solid particles in hexamethyldisilazane are trapped on the medium, thereby realizing the operation of solid-liquid separation, and removing the particles in hexamethyldisilazane, thereby obtaining electronic-grade hexamethyldisilazane.
Further, the step S4 further includes the following steps:
s4.1, before the electronic-grade hexamethyldisilazane is sent into the product tank 13, a first valve 18 of a pipeline where a feed inlet of the product tank 13 is positioned is closed, a third valve 20 of a pipeline where a discharge outlet of the bottom of the product tank 13 is positioned is opened, a second valve 19 of a pipeline where an extraction outlet of the top of the product tank 13 is positioned is opened, and a vacuum pump 17 works to generate negative pressure, so that the vacuum state is kept in the product tank 13 and the sampling tank 15, and meanwhile, waste gas in the product tank 13 and the sampling tank 15 is sucked into the vacuum tank 16, and then the second valve 19 and the third valve 20 are closed; in addition, the hexamethyldisilazane is also protected by nitrogen before entering the product tank 13, so that the purification is further prevented from being influenced by byproducts generated by raw material hydrolysis.
S4.2, opening a first valve 18, and allowing materials to enter the product tank 13;
and S4.3, when sampling is needed, opening the third valve 20, and allowing the material to enter the sampling box 15 from the product tank 13. After the design, the vacuum state is kept in the product tank 13 and the sampling box 15, so that the products subjected to resin adsorption and filtration and impurity removal are not contacted with moisture in the air when being filled, and meanwhile, the collected samples can be prevented from being hydrolyzed, and the sampling accuracy is ensured.
In order to verify the effect of the invention on hexamethyldisilazane purification, a correlation test analysis procedure was performed as follows:
1. hexamethyldisilazane was analyzed by coulombic method karl fischer moisture meter, GC-MS, LPC and ICP-MS, and its moisture, composition, particle size and metal ion information and its content are shown in tables 1 to 4.
TABLE 1 moisture content of hexamethyldisilazane
TABLE 2 hexamethyldisilazane composition information
The gas chromatograph-mass spectrometer for detection is equipped with a FID detector, a DB-1ms ultra-high inert column and a DB-1701 column, and the component content information is obtained by normalizing the chromatographic peak area.
TABLE 3 hexamethyldisilazane particle size
TABLE 4 hexamethyldisilazane Metal ion content information
| Ag(μg/kg) | Al(μg/kg) | As(μg/kg) | Au(μg/kg) | B(μg/kg) | Ba(μg/kg) |
| ＜1 | 3 | ＜1 | ＜1 | 394 | ＜1 |
| Be(μg/kg) | Ca(μg/kg) | Cd(μg/kg) | Co(μg/kg) | Cr(μg/kg) | Cu(μg/kg) |
| ＜0.1 | ＜1 | ＜1 | ＜1 | ＜1 | 670 |
| Fe(μg/kg) | Hg(μg/kg) | K(μg/kg) | Li(μg/kg) | Mg(μg/kg) | Mn(μg/kg) |
| ＜5 | ＜1 | 2 | ＜1 | ＜1 | 9 |
| Na(μg/kg) | Ni(μg/kg) | Pb(μg/kg) | Sn(μg/kg) | Sr(μg/kg) | Zn(μg/kg) |
| ＜1 | 29 | ＜1 | ＜1 | 1 | ＜1 |
| Tl(μg/kg) | In(μg/kg) | Bi(μg/kg) | Zr(μg/kg) | Ti(μg/kg) | Mo(μg/kg) |
| <1 | <1 | <1 | 1 | 388 | <1 |
As can be seen from Table 1, the moisture content of the raw material was relatively high, the average value was 1553ppm, and the moisture was removed by adsorption on silica gel and rectification. As can be seen from Table 2, the components other than hexamethyldisilazane are very small in content, and the impurity components can be completely removed by the rectification and purification steps to obtain electronic grade hexamethyldisilazane. As can be seen from tables 3 and 4, the hexamethyldisilazane component has a large amount of particles and metal ion impurities, and the metal ion and the particulate impurities can be further removed by the resin adsorption system and the filtration system to obtain electronic grade hexamethyldisilazane.
2. The purification process of the hexamethyldisilazane by the device and the purification method thereof is as follows:
as shown in Table 5, after the hexamethyldisilazane is subjected to the silica gel adsorption and rectification treatment, the moisture content in the sample is obviously reduced, the average value is 16ppm, and the silica gel adsorption and rectification treatment can remove the moisture in the sample.
TABLE 5 moisture content of hexamethyldisilazane after removal of impurities by adsorption
As shown in Table 6, after the impurity removal by rectification of hexamethyldisilazane, the content of hexamethyldisilazane in the sample reaches more than 99.99%, and the impurities of hexamethyldisiloxane and trimethylsilanol can be removed by the step of impurity removal by rectification.
TABLE 6 hexamethyldisilazane composition information after removal of impurities by rectification
The rectification system is communicated with the resin adsorption system (11) as shown in fig. 1, the heavy removal rectification tower (7) is communicated with the resin adsorption system (11) and the filtration system (12) as shown in fig. 1, and hexamethyldisilazane materials in the rectification storage tank are conveyed to the resin adsorption system (11) and the filtration system (12) by a feed pump, and metal ions and particulate impurity components are removed in the hexamethyldisilazane materials.
As shown in tables 7 and 8, after impurity removal by the adsorption system and the filtration system, the content of metal ions and particulate impurities in the hexamethyldisilazane in the sample is obviously reduced, and the impurities can be removed by the adsorption system and the filtration system, so that the requirements of electronic-grade hexamethyldisilazane are finally met.
TABLE 7 hexamethyldisilazane Metal ion content information after removal of impurities by adsorption apparatus
| Ag(μg/kg) | Al(μg/kg) | As(μg/kg) | Au(μg/kg) | B(μg/kg) | Ba(μg/kg) |
| ＜1 | ＜1 | ＜1 | ＜1 | ＜1 | ＜1 |
| Be(μg/kg) | Ca(μg/kg) | Cd(μg/kg) | Co(μg/kg) | Cr(μg/kg) | Cu(μg/kg) |
| ＜1 | ＜1 | ＜1 | ＜1 | ＜1 | ＜1 |
| Fe(μg/kg) | Hg(μg/kg) | K(μg/kg) | Li(μg/kg) | Mg(μg/kg) | Mn(μg/kg) |
| ＜1 | ＜1 | ＜1 | ＜1 | ＜1 | ＜1 |
| Na(μg/kg) | Ni(μg/kg) | Pb(μg/kg) | Sn(μg/kg) | Sr(μg/kg) | Zn(μg/kg) |
| ＜1 | ＜1 | ＜1 | ＜1 | ＜1 | ＜1 |
| Tl(μg/kg) | In(μg/kg) | Bi(μg/kg) | Zr(μg/kg) | Ti(μg/kg) | Mo(μg/kg) |
| ＜1 | ＜1 | ＜1 | ＜1 | ＜1 | ＜1 |
TABLE 8 hexamethyldisilazane particle size after removal of impurities by filtration apparatus
The foregoing embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the present invention, and the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without collision. The protection scope of the present invention is defined by the claims, and the protection scope includes equivalent alternatives to the technical features of the claims. I.e., equivalent replacement modifications within the scope of this invention are also within the scope of the invention.
Claims (9)
1. The utility model provides an electronic grade hexamethyldisilazane purification device, includes raw materials storage tank (1), raw materials storage tank (1) discharge gate passes through the pipeline and is connected with light removal rectifying column (4) feed end, light removal rectifying column (4) bottom discharge gate passes through the pipeline and is connected with heavy removal rectifying column (7) feed inlet, light removal rectifying column (4) top gas outlet passes through pipeline and first condenser (5) access connection, first condenser (5) export passes through the pipeline and is connected with waste storage tank (6), light removal rectifying column (7) top gas outlet passes through pipeline and is connected with second condenser (8) access connection, second condenser (8) export passes through the pipeline and is connected with rectification storage tank (9) feed inlet, its characterized in that: the discharge port of the rectification storage tank (9) is connected with the feed port of the resin adsorption system (11) through a pipeline, the discharge port of the resin adsorption system (11) is connected with the feed port of the filtration system (12) through a pipeline, and the discharge port of the filtration system (12) is connected with the feed port of the product tank (13) through a pipeline.
2. An electronic grade hexamethyldisilazane purification unit according to claim 1, wherein: the top extraction opening of the product tank (13) is connected with one end of a vacuum tank (16) through a pipeline, and the other end of the vacuum tank (16) is connected with a vacuum pump (17) through a pipeline.
3. An electronic grade hexamethyldisilazane purification unit according to claim 2, wherein: the bottom discharge port of the product tank (13) is connected with one end of a product pump (14) through a pipeline, and the other end of the product pump (14) is connected with a sampling box (15) through a pipeline.
4. An electronic grade hexamethyldisilazane purification unit of claim 3, wherein: the pipeline at the feed inlet of the product tank (13) is provided with a first valve (18), the pipeline at the extraction opening at the top of the product tank (13) is provided with a second valve (19), and the pipeline at the discharge outlet at the bottom of the product tank (13) is provided with a third valve (20).
5. An electronic grade hexamethyldisilazane purification unit according to claim 1, wherein: the silica gel adsorption system is characterized in that a silica gel adsorption system (2) is arranged on a pipeline where a feed inlet of the raw material storage tank (1) is located, and a first feed pump (3) is arranged on a pipeline between a discharge outlet of the raw material storage tank (1) and a feed inlet of the light component removal rectifying tower (4).
6. An electronic grade hexamethyldisilazane purification unit according to claim 1, wherein: and a second feed pump (10) is arranged on a pipeline between the discharge port of the rectification storage tank (9) and the feed port of the resin adsorption system (11).
7. An electronic grade hexamethyldisilazane purification unit according to claim 1, wherein: the adsorbent adopted by the resin adsorption system (11) is cation exchange resin, and the filtering precision of the filter element selected by the filtering system (12) is 0.02 mu m.
8. A purification method of the electronic grade hexamethyldisilazane purification device according to any one of claims 1 to 7, characterized in that: it comprises the following steps:
s1: raw materials enter a silica gel adsorption system (2) through a pipeline, are subjected to silica gel adsorption treatment to remove part of water, and are pumped into a raw material storage tank (1);
s2: the materials in the raw material storage tank (1) sequentially pass through a light removal rectifying tower (4) and a heavy removal rectifying tower (7) for rectification, light components-trimethylsilanol and hexamethyldisilazane in the industrial-grade hexamethyldisilazane are separated through the light removal rectifying tower (4), and heavy components-metal impurities and partial particles in the industrial-grade hexamethyldisilazane are separated through the heavy removal rectifying tower (7); then the materials are sent into a rectification storage tank (9);
s3: the material in the rectifying storage tank (9) passes through a resin adsorption system (11) and utilizes ion exchange resin to exchange cations in hexamethyldisilazane, so that the cations in the material are transferred to the resin, and the aim of desalting is fulfilled;
s4: the materials treated by the resin adsorption system (11) enter a filtering system (12), and solid particles in hexamethyldisilazane are trapped on the materials, so that the operation of solid-liquid separation is realized; removing particles in hexamethyldisilazane to obtain electronic grade hexamethyldisilazane, and delivering the electronic grade hexamethyldisilazane into a product tank (13).
9. The purification method of the electronic grade hexamethyldisilazane purification device according to claim 8, wherein: the step S4 further includes the steps of:
s4.1, before the electronic-grade hexamethyldisilazane is sent into a product tank (13), a first valve (18) of a pipeline where a feed inlet of the product tank (13) is positioned is closed, a third valve (20) of a pipeline where a discharge outlet of the bottom of the product tank (13) is positioned is opened, a second valve (19) of a pipeline where an extraction opening of the top of the product tank (13) is positioned is opened, a vacuum pump (17) works to generate negative pressure, so that the vacuum state is kept in the product tank (13) and a sampling box (15), waste gas in the product tank (13) and the sampling box (15) is sucked into a vacuum tank (16), and then the second valve (19) and the third valve (20) are closed;
s4.2, opening a first valve (18), and enabling materials to enter a product tank (13);
and S4.3, when sampling is needed, opening a third valve (20), and allowing materials to enter the sampling box (15) from the product tank (13).
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