CN111205168A - Method for producing ultra-high-purity isopropanol by using resin purification method - Google Patents

Method for producing ultra-high-purity isopropanol by using resin purification method Download PDF

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CN111205168A
CN111205168A CN202010116289.9A CN202010116289A CN111205168A CN 111205168 A CN111205168 A CN 111205168A CN 202010116289 A CN202010116289 A CN 202010116289A CN 111205168 A CN111205168 A CN 111205168A
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isopropanol
resin
column
purity
mixed resin
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高小云
赵俊男
刘兵
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Suzhou Crystal Clear Chemical Co ltd
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    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
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Abstract

The invention discloses a method for producing ultrahigh-purity isopropanol by using a resin purification method, which comprises the following steps: (1) introducing gas into a drying column, drying, and introducing the dried gas into an isopropanol raw material tank; (2) communicating an isopropanol raw material tank with a power pump, introducing the isopropanol raw material in an isopropanol raw material tank column into a purification pipeline by the power pump by taking gas as a carrier, and introducing the isopropanol raw material into a mixed resin exchange column through the purification pipeline; (3) adjusting the pressure and flow rate of isopropanol introduced into the mixed resin exchange column, and purifying the isopropanol through the mixed resin exchange column to obtain ultrahigh-purity isopropanol; (4) ultra-high purity isopropanol enters the product storage tank via an outlet line. The method uses gas as a carrier to introduce the isopropanol into a specially designed mixed resin exchange column so as to remove metal cation impurities and anion impurities in the isopropanol, greatly simplifies the purification process flow, can produce ultrahigh-purity isopropanol on a large scale, and has low production energy consumption and low production cost.

Description

Method for producing ultra-high-purity isopropanol by using resin purification method
Technical Field
The invention belongs to the technical field of isopropanol purification, and particularly relates to a method for producing ultrahigh-purity isopropanol by using a resin purification method.
Background
Ultra-high purity isopropanol has been widely used in the cleaning process of each stage of ultra-clean monocrystalline silicon wafers of semiconductors. In semiconductor manufacturing processes, the silicon wafer surface must be cleaned and dried sufficiently after each step in order to improve yield. The participation of various aqueous solutions inevitably required in various processes of semiconductor production causes that water is continuously accumulated on the surface of the silicon wafer in the production, various ions are usually accumulated in the water to form a solution, and therefore, metal salt stains are inevitably remained on the surface of the silicon wafer in the drying process, which is fatal to the next high-precision semiconductor production process. In addition, various organic substances are accumulated on the surface of the silicon wafer. Therefore, the surface of the silicon wafer needs to be cleaned with isopropyl alcohol.
Because the isopropanol has good volatility and water intersolubility, salt solution, organic impurities, particle impurities and the like remained on the surface of the silicon wafer after the processes of all stages of the monocrystalline silicon wafer are effectively mixed with the isopropanol and taken away along with the flow of the isopropanol. And finally, residual isopropanol volatilizes, so that the silicon wafer can be ensured to be in a clean and dry state quickly, and the silicon wafer can be ensured not to have flaws and dead spots due to the influence of surface metal salts and the like in the next process, thereby improving the yield. Isopropyl alcohol is an extremely large and indispensable cleaning agent in the semiconductor manufacturing process.
In recent years, with the rapid miniaturization of chip threads, the highest precision of chips has reached 7nm of processes; since the semiconductor itself is too fine, the isopropyl alcohol for cleaning itself is required to have a sufficient purity, a sufficiently low metal ion content, and a sufficiently low moisture content and other organic matter content. However, in actual use, the impurity metals and anions in isopropanol exceed SEMI C12 standards, thus presenting a significant challenge to isopropanol purification.
At present, most of ultra-high purity isopropanol produced in China adopts a distillation method to remove metal ions dissolved in the isopropanol. For example, patent CN102452897 and patent CN 102898275 are rectified by a distillation tower and a rectification tower, and then condensed by a condenser to form liquid high-purity isopropanol. However, the method has overlarge energy consumption, is not beneficial to long-term development, and the production process is too complicated and precise because the isopropanol and the water form an azeotrope, so that the stability of the product cannot be ensured. In patent CN106748652, natural fiber treated by chemical modification is used as adsorbent of trace metal ions in isopropanol, and then ion exchange is performed by using cation exchange column, so that the impurity metal ions in the finally obtained isopropanol are less than 0.1ppb, and no data exists in anions. Patent CN103613486 is prepared by adding metal salt chelate, and filtering by anion exchange resin, cation exchange resin, molecular sieve, water-absorbing resin, multi-stage continuous rectification device and nanofiltration membrane respectively to obtain ultrapure isopropanol; the obtained ultrapure isopropanol has a cation content of less than 0.1ppb and an anion content of less than 50 ppb; the method has the disadvantages of long process, high energy consumption in actual production, and difficult control.
In conclusion, the published and reported isopropanol purification technology mainly focuses on distillation-rectification technology, which has strict requirements on equipment materials, and consumes a large amount of steam and electric energy in the purification process.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for producing ultrahigh-purity isopropanol by using a resin purification method, which uses gas as a carrier to introduce isopropanol into a specially designed mixed resin exchange column so as to remove metal cation impurities and anion impurities in the isopropanol, greatly simplifies the purification process flow, can produce ultrahigh-purity isopropanol in a large scale, and has low production energy consumption and low production cost.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a method for producing ultra-high purity isopropanol by using a resin purification method comprises the following steps:
(1) introducing gas into a drying column, drying, and introducing the dried gas into an isopropanol raw material tank through a pipeline;
(2) communicating an isopropanol raw material tank with a power pump, introducing the isopropanol raw material in an isopropanol raw material tank column into a purification pipeline by the power pump by taking gas as a carrier, and introducing the isopropanol raw material into a mixed resin exchange column through the purification pipeline;
(3) adjusting the pressure and flow rate of isopropanol introduced into the mixed resin exchange column, and purifying the isopropanol through the mixed resin exchange column to obtain ultrahigh-purity isopropanol;
(4) ultra-high purity isopropanol enters the product storage tank via an outlet line.
Further, the gas in the step (1) is nitrogen gas, air or ultra-pure nitrogen gas.
Further, the drying column in the step (1) is filled with a 3A-grade molecular sieve.
Further, the length of the drying column is 1.5-2.5 times of the length of the mixed resin exchange column.
Further, the mixed resin exchange column is filled with mixed bed resin formed by mixing anion exchange resin and cation exchange resin, and the mixed bed resin is prepared by sequentially treating the mixed resin formed by mixing anion exchange resin and cation exchange resin with high-purity water, high-purity ethanol, high-purity sodium hydroxide and high-purity hydrochloric acid, washing with high-purity water and finally exposing and irradiating by ultraviolet light.
Furthermore, the volume ratio of the cation exchange resin to the anion exchange resin in the mixed resin exchange column is 1: 1-n: 1, and n is more than 1.
Further, the mixed resin exchange column is cylindrical, and the ratio of the column height to the column diameter is 15: 1.
Further, the mixed resin exchange column has two ports for connecting the purge line and the outlet line, and the ratio of the diameter of the ports to the diameter of the column of the mixed resin exchange column is 1: 2.
Further, the purification temperature of the mixed resin exchange column is 25 ℃ +/-5 ℃.
Furthermore, the pressure of the isopropanol led into the mixed resin exchange column is 1.05-1.15 atmospheric pressures, and the flow rate of the isopropanol led into the mixed resin exchange column is 240-360 times of the volume of the mixed bed resin per hour.
The invention has the beneficial effects that:
the invention uses the isopropanol with low water content after the industrial grade isopropanol is dehydrated as the raw material, the isopropanol with low water content flows through the mixed resin exchange column which is specially designed and manufactured by the agitation of the drying gas and the pressure supplied by the power pump to remove the metal ions and the anions which are impurities, after the purification, the metal ions are less than 5ppt, and the anions are less than 1 ppb.
The method does not adopt a distillation-rectification process, but uses dry gas as a carrier to introduce isopropanol into a mixed resin exchange column for purification treatment; the mixed resin exchange column is filled with mixed bed resin formed by mixing anion exchange resin and cation exchange resin, the mixed bed resin is prepared by sequentially treating the mixed resin formed by mixing the anion exchange resin and the cation exchange resin with high-purity water, high-purity ethanol, high-purity sodium hydroxide and high-purity hydrochloric acid, washing with high-purity water and finally exposing and irradiating by ultraviolet light; the mixed resin exchange column manufactured in the way can effectively remove metal ion impurities and anion impurities in isopropanol at the same time without other complex processes;
after the isopropanol is introduced into the mixed resin exchange column, the adsorption capacity of the mixed bed resin in the mixed resin exchange column on metal ions and anions is improved by adjusting the pressure and flow rate of the introduced isopropanol.
The method is simple to operate, has extremely low energy consumption, and can realize stable and reliable large-scale industrial production of the electronic grade isopropanol.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, inductively coupled plasma mass spectrometry (model: ICP-MS8900) was used to detect the metal ion content, an anion chromatograph (Thermo Fisher AQ model) was used to detect the anion content, and a Metter V20 trace moisture tester was used to detect the moisture content.
Example 1
In this example 1, the length of the drying column was 1.5 times the length of the mixed resin exchange column, and the drying column was filled with a 3A-grade molecular sieve;
the mixed resin exchange column is filled with mixed bed resin formed by mixing anion exchange resin and cation exchange resin, wherein the volume ratio of the cation exchange resin to the anion exchange resin is 1: 1; the mixed bed resin is prepared by sequentially treating mixed resin obtained by mixing anion exchange resin and cation exchange resin with high-purity water, high-purity ethanol, high-purity sodium hydroxide and high-purity hydrochloric acid, washing with high-purity water, and finally exposing and irradiating with ultraviolet light.
In this example 1, the mixed resin exchange column was cylindrical with a ratio of column height to column diameter of 15: 1; the ratio of the diameter of the two connectors of the mixed resin exchange column for connecting the purifying pipeline and the output pipeline to the cylinder diameter of the mixed resin exchange column is 1: 2. The packed volume of the mixed bed resin in the mixed resin exchange column is 50% of the volume of the mixed resin exchange column, and the purification temperature in the mixed resin exchange column is 25 ℃.
The purification pipeline and the output pipeline connected with the mixed resin exchange column are stainless steel pipelines, and the lining is made of PFA material. Three-way valves are arranged on the purification pipeline and the output pipeline.
The process for producing ultra-high purity isopropyl alcohol of example 1, comprising the steps of:
(1) introducing nitrogen into a drying column for drying, and introducing the nitrogen dried by a molecular sieve into an isopropanol stock tank through a pipeline;
(2) communicating an isopropanol raw material tank with a power pump, introducing the isopropanol raw material in an isopropanol raw material tank column into a purification pipeline by the power pump by taking nitrogen as a carrier, and introducing the isopropanol raw material into a mixed resin exchange column through the purification pipeline;
(3) adjusting the pressure and flow rate of isopropanol led into the mixed resin exchange column through a three-way valve, maintaining the pressure in the mixed resin exchange column to be 1.05 atmospheric pressure, and the flow rate of the isopropanol to be 300 times of the volume of the mixed bed resin per hour, and purifying the isopropanol through the mixed resin exchange column to obtain ultrahigh-purity isopropanol;
(4) the ultra-high purity isopropanol enters a product storage tank through an output pipeline, waits for filling, and is sampled and detected; the results of metal ion content measurement are shown in table 1, the results of anion content measurement are shown in table 2, and the results of moisture content measurement are shown in table 3.
TABLE 1 results of metal ion content measurement
Figure BDA0002391598540000061
Figure BDA0002391598540000071
TABLE 2 anion content test results
Figure BDA0002391598540000072
TABLE 3 moisture content test results
Figure BDA0002391598540000073
Example 2
In this example 2, the length of the drying column was 2.5 times the length of the mixed resin exchange column, and the drying column was filled with a 3A-grade molecular sieve;
the mixed resin exchange column is filled with mixed bed resin formed by mixing anion exchange resin and cation exchange resin, wherein the volume ratio of the cation exchange resin to the anion exchange resin is 1: 1; the mixed bed resin is prepared by sequentially treating mixed resin obtained by mixing anion exchange resin and cation exchange resin with high-purity water, high-purity ethanol, high-purity sodium hydroxide and high-purity hydrochloric acid, washing with high-purity water, and finally exposing and irradiating with ultraviolet light.
In this example 2, the mixed resin exchange column was cylindrical with a ratio of column height to column diameter of 15: 1; the ratio of the diameter of the two connectors of the mixed resin exchange column for connecting the purifying pipeline and the output pipeline to the cylinder diameter of the mixed resin exchange column is 1: 2. The packed volume of the mixed bed resin in the mixed resin exchange column is 75% of the volume of the mixed resin exchange column, and the purification temperature in the mixed resin exchange column is 25 ℃.
The purification pipeline and the output pipeline connected with the mixed resin exchange column are stainless steel pipelines, and the lining is made of PFA material. Three-way valves are arranged on the purification pipeline and the output pipeline.
The process for producing ultra-high purity isopropyl alcohol of example 2, comprising the steps of:
(1) introducing nitrogen into a drying column for drying, and introducing the nitrogen dried by a molecular sieve into an isopropanol stock tank through a pipeline;
(2) communicating an isopropanol raw material tank with a power pump, introducing the isopropanol raw material in an isopropanol raw material tank column into a purification pipeline by the power pump by taking nitrogen as a carrier, and introducing the isopropanol raw material into a mixed resin exchange column through the purification pipeline;
(3) adjusting the pressure and flow rate of isopropanol led into the mixed resin exchange column through a three-way valve, maintaining the pressure in the mixed resin exchange column to be 1.15 atmospheric pressures, wherein the flow rate of the isopropanol is 240 times of the volume of the mixed bed resin per hour, and purifying the isopropanol through the mixed resin exchange column to obtain ultrahigh-purity isopropanol;
(4) the ultra-high purity isopropanol enters a product storage tank through an output pipeline, waits for filling, and is sampled and detected; the results of metal ion content measurement are shown in table 4, the results of anion content measurement are shown in table 5, and the results of moisture content measurement are shown in table 6.
TABLE 4 results of metal ion content measurement
Figure BDA0002391598540000091
TABLE 5 anion content measurement results
Figure BDA0002391598540000092
TABLE 6 moisture content test results
Figure BDA0002391598540000101
Example 3
In this example 3, the length of the drying column was 1.5 times the length of the mixed resin exchange column, and the drying column was filled with a 3A-grade molecular sieve;
the mixed resin exchange column is filled with mixed bed resin formed by mixing anion exchange resin and cation exchange resin, wherein the volume ratio of the cation exchange resin to the anion exchange resin is 1: 1; the mixed bed resin is prepared by sequentially treating mixed resin obtained by mixing anion exchange resin and cation exchange resin with high-purity water, high-purity ethanol, high-purity sodium hydroxide and high-purity hydrochloric acid, washing with high-purity water, and finally exposing and irradiating with ultraviolet light.
In this example 3, the mixed resin exchange column was cylindrical with a ratio of column height to column diameter of 15: 1; the ratio of the diameter of the two connectors of the mixed resin exchange column for connecting the purifying pipeline and the output pipeline to the cylinder diameter of the mixed resin exchange column is 1: 2. The packed volume of the mixed bed resin in the mixed resin exchange column is 50% of the volume of the mixed resin exchange column, and the purification temperature in the mixed resin exchange column is 25 ℃.
The purification pipeline and the output pipeline connected with the mixed resin exchange column are stainless steel pipelines, and the lining is made of PFA material. Three-way valves are arranged on the purification pipeline and the output pipeline.
The process for producing ultra-high purity isopropyl alcohol of example 3, comprising the steps of:
(1) introducing nitrogen into a drying column for drying, and introducing the nitrogen dried by a molecular sieve into an isopropanol stock tank through a pipeline;
(2) communicating an isopropanol raw material tank with a power pump, introducing the isopropanol raw material in an isopropanol raw material tank column into a purification pipeline by the power pump by taking nitrogen as a carrier, and introducing the isopropanol raw material into a mixed resin exchange column through the purification pipeline;
(3) adjusting the pressure and flow rate of isopropanol led into the mixed resin exchange column through a three-way valve, maintaining the pressure in the mixed resin exchange column to be 1.05 atmospheric pressure, and the flow rate of the isopropanol to be 360 times of the volume of the mixed bed resin per hour, and purifying the isopropanol through the mixed resin exchange column to obtain ultrahigh-purity isopropanol;
(4) the ultra-high purity isopropanol enters a product storage tank through an output pipeline, waits for filling, and is sampled and detected; the results of metal ion content measurement are shown in table 7, the results of anion content measurement are shown in table 8, and the results of moisture content measurement are shown in table 9.
TABLE 7 results of metal ion content measurement
Figure BDA0002391598540000111
Figure BDA0002391598540000121
TABLE 8 anion content measurement results
Figure BDA0002391598540000122
TABLE 9 moisture content test results
Figure BDA0002391598540000123
Example 4
In this example 4, the length of the drying column was 1.5 times the length of the mixed resin exchange column, and the drying column was filled with a 3A grade molecular sieve;
the mixed resin exchange column is filled with mixed bed resin formed by mixing anion exchange resin and cation exchange resin, wherein the volume ratio of the cation exchange resin to the anion exchange resin is 1: 1; the mixed bed resin is prepared by sequentially treating mixed resin obtained by mixing anion exchange resin and cation exchange resin with high-purity water, high-purity ethanol, high-purity sodium hydroxide and high-purity hydrochloric acid, washing with high-purity water, and finally exposing and irradiating with ultraviolet light.
In this example 4, the mixed resin exchange column was cylindrical with a ratio of column height to column diameter of 15: 1; the ratio of the diameter of the two connectors of the mixed resin exchange column for connecting the purifying pipeline and the output pipeline to the cylinder diameter of the mixed resin exchange column is 1: 2. The packed volume of the mixed bed resin in the mixed resin exchange column is 50% of the volume of the mixed resin exchange column, and the purification temperature in the mixed resin exchange column is 25 ℃.
The purification pipeline and the output pipeline connected with the mixed resin exchange column are stainless steel pipelines, and the lining is made of PFA material. Three-way valves are arranged on the purification pipeline and the output pipeline.
The process for producing ultra-high purity isopropyl alcohol of example 4, comprising the steps of:
(1) introducing nitrogen into a drying column for drying, and introducing the nitrogen dried by a molecular sieve into an isopropanol stock tank through a pipeline;
(2) communicating an isopropanol raw material tank with a power pump, introducing the isopropanol raw material in an isopropanol raw material tank column into a purification pipeline by the power pump by using nitrogen as a carrier, and sequentially introducing two mixed resin exchange columns connected in series through the purification pipeline (the two mixed resin exchange columns are the mixed resin exchange columns with the same specification prepared in example 4);
(3) adjusting the pressure and flow rate of isopropanol led into the mixed resin exchange column through a three-way valve, maintaining the pressure in the mixed resin exchange column to be 1.05 atmospheric pressure, and the flow rate of the isopropanol to be 300 times of the volume of the mixed bed resin per hour, and purifying the isopropanol through the mixed resin exchange column to obtain ultrahigh-purity isopropanol;
(4) the ultra-high purity isopropanol enters a product storage tank through an output pipeline, waits for filling, and is sampled and detected; the results of metal ion content measurement are shown in table 10, the results of anion content measurement are shown in table 11, and the results of moisture content measurement are shown in table 12.
TABLE 10 results of metal ion content measurement
Figure BDA0002391598540000131
Figure BDA0002391598540000141
TABLE 11 anion content measurement results
Figure BDA0002391598540000142
TABLE 12 moisture content test results
Figure BDA0002391598540000143
Example 5
In this example 5, the length of the drying column was 2 times the length of the mixed resin exchange column, and the drying column was filled with a 3A grade molecular sieve;
the mixed resin exchange column is filled with mixed bed resin formed by mixing anion exchange resin and cation exchange resin, wherein the volume ratio of the cation exchange resin to the anion exchange resin is 1: 1; the mixed bed resin is prepared by sequentially treating mixed resin obtained by mixing anion exchange resin and cation exchange resin with high-purity water, high-purity ethanol, high-purity sodium hydroxide and high-purity hydrochloric acid, washing with high-purity water, and finally exposing and irradiating with ultraviolet light.
In this example 5, the mixed resin exchange column was cylindrical with a ratio of column height to column diameter of 15: 1; the ratio of the diameter of the two connectors of the mixed resin exchange column for connecting the purifying pipeline and the output pipeline to the cylinder diameter of the mixed resin exchange column is 1: 2. The packed volume of the mixed bed resin in the mixed resin exchange column is 75% of the volume of the mixed resin exchange column, and the purification temperature in the mixed resin exchange column is 25 ℃.
The purification pipeline and the output pipeline connected with the mixed resin exchange column are stainless steel pipelines, and the lining is made of PFA material. Three-way valves are arranged on the purification pipeline and the output pipeline.
The process for producing ultra-high purity isopropyl alcohol of example 5, comprising the steps of:
(1) introducing nitrogen into a drying column for drying, and introducing the nitrogen dried by a molecular sieve into an isopropanol stock tank through a pipeline;
(2) communicating an isopropanol raw material tank with a power pump, introducing the isopropanol raw material in an isopropanol raw material tank column into a purification pipeline by the power pump by using nitrogen as a carrier, and sequentially introducing two mixed resin exchange columns connected in series through the purification pipeline (the two mixed resin exchange columns are the mixed resin exchange columns with the same specification prepared in example 5);
(3) adjusting the pressure and flow rate of isopropanol led into the mixed resin exchange column through a three-way valve, maintaining the pressure in the mixed resin exchange column to be 1.15 atmospheric pressures, wherein the flow rate of the isopropanol is 240 times of the volume of the mixed bed resin per hour, and purifying the isopropanol through the mixed resin exchange column to obtain ultrahigh-purity isopropanol;
(4) the ultra-high purity isopropanol enters a product storage tank through an output pipeline, waits for filling, and is sampled and detected; the results of metal ion content measurement are shown in table 13, the results of anion content measurement are shown in table 14, and the results of moisture content measurement are shown in table 15.
TABLE 13 measurement results of the content of metal ions
Figure BDA0002391598540000161
Figure BDA0002391598540000171
TABLE 14 anion content measurement results
Figure BDA0002391598540000172
TABLE 15 moisture content test results
Figure BDA0002391598540000173
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents made by the contents of the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.

Claims (10)

1. A method for producing ultrahigh-purity isopropanol by using a resin purification method is characterized by comprising the following steps:
(1) introducing gas into a drying column, drying, and introducing the dried gas into an isopropanol raw material tank through a pipeline;
(2) communicating an isopropanol raw material tank with a power pump, introducing the isopropanol raw material in an isopropanol raw material tank column into a purification pipeline by the power pump by taking gas as a carrier, and introducing the isopropanol raw material into a mixed resin exchange column through the purification pipeline;
(3) adjusting the pressure and flow rate of isopropanol introduced into the mixed resin exchange column, and purifying the isopropanol through the mixed resin exchange column to obtain ultrahigh-purity isopropanol;
(4) ultra-high purity isopropanol enters the product storage tank via an outlet line.
2. The method for producing ultra-high purity isopropyl alcohol according to claim 1, wherein the gas in the step (1) is nitrogen or air.
3. The method for producing ultra-high purity isopropyl alcohol according to claim 1, wherein the drying column in the step (1) is filled with a molecular sieve.
4. The method for producing ultrahigh-purity isopropanol by using the resin purification method as claimed in claim 1, wherein the length of the drying column is 1.5 to 2.5 times the length of the mixed resin exchange column.
5. The method for producing ultrahigh-purity isopropanol by using the resin purification method as claimed in claim 1, wherein the mixed resin exchange column is filled with a mixed bed resin formed by mixing anion exchange resin and cation exchange resin, and the mixed bed resin is prepared by sequentially treating the mixed resin formed by mixing anion exchange resin and cation exchange resin with high-purity water, high-purity ethanol, high-purity sodium hydroxide and high-purity hydrochloric acid, washing with high-purity water, and finally exposing and irradiating with ultraviolet light.
6. The method for producing ultra-high purity isopropyl alcohol according to claim 5, wherein: the volume ratio of the cation exchange resin to the anion exchange resin in the mixed resin exchange column is 1: 1-n: 1, and n is more than 1.
7. The method for producing ultra-high purity isopropyl alcohol according to claim 1, wherein: the mixed resin exchange column is cylindrical, and the ratio of the height of the column body to the diameter of the column body is 15: 1.
8. The method for producing ultra-high purity isopropyl alcohol according to claim 1, wherein: the mixed resin exchange column has two ports for connecting the purification pipeline and the output pipeline, and the ratio of the port diameter to the column diameter of the mixed resin exchange column is 1: 2.
9. The method for producing ultra-high purity isopropyl alcohol according to claim 1, wherein: the purification temperature of the mixed resin exchange column is 25 +/-5 ℃.
10. The method for producing ultra-high purity isopropyl alcohol according to claim 5, wherein: the pressure of the isopropanol led into the mixed resin exchange column is 1.05-1.15 atmospheric pressures, and the flow rate of the isopropanol led into the mixed resin exchange column is 240-360 times of the volume of the mixed bed resin per hour.
CN202010116289.9A 2020-02-25 2020-02-25 Method for producing ultra-high-purity isopropanol by using resin purification method Pending CN111205168A (en)

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CN114470958A (en) * 2022-02-15 2022-05-13 北京袭明科技有限公司 Production method and device of high-purity electronic grade methanol
CN115322074A (en) * 2022-07-06 2022-11-11 晶瑞(湖北)微电子材料有限公司 Purification method of isopropanol
WO2023102727A1 (en) * 2021-12-07 2023-06-15 晶瑞电子材料股份有限公司 Method for producing ultra-high purity isopropanol by using resin purification method

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