阅读说明：本技术 超纯异丙醇溶液的制备方法及其微量丙酮的去除方法 (Preparation method of ultrapure isopropanol solution and method for removing trace acetone of ultrapure isopropanol solution ) 是由 曹传兴 毕亚群 吴国新 于 2020-10-15 设计创作，主要内容包括：本发明公开了一种异丙醇溶液中微量丙酮的去除方法,采用碱性固体颗粒物做为吸附剂去除异丙醇溶液中丙酮,所述吸附剂的主要成分包括活性氧化铝、亚硫酸氢钠,高锰酸钾,粘合剂和发泡剂。本发明还公开了一种超纯异丙醇溶液的制备方法,具体步骤包括：S1、去除丙酮：采用上述的丙酮的去除方法,得到去除丙酮后的异丙醇溶液；S2、离子去除：所述去除丙酮后的异丙醇溶液进入离子吸附罐,得到去除金属离子后的异丙醇溶液；S3、精馏：所述去除金属离子后的异丙醇溶液进入精馏塔精馏,获得满足半导体芯片级的异丙醇溶液产品。本发明超纯异丙醇溶液的制备方法及其微量丙酮的去除方法,工艺简单适合工业化,丙酮去除率高,成本低廉。(The invention discloses a method for removing trace acetone in an isopropanol solution, which adopts alkaline solid particles as an adsorbent to remove acetone in the isopropanol solution, wherein the main components of the adsorbent comprise active aluminum oxide, sodium bisulfite, potassium permanganate, an adhesive and a foaming agent. The invention also discloses a preparation method of the ultrapure isopropanol solution, which comprises the following specific steps: s1, removing acetone: the isopropanol solution after the acetone is removed is obtained by adopting the acetone removal method; s2, ion removal: the isopropanol solution after the acetone removal enters an ion adsorption tank to obtain the isopropanol solution after the metal ions are removed; s3, rectification: and the isopropanol solution after the metal ions are removed enters a rectifying tower for rectification to obtain an isopropanol solution product meeting the semiconductor chip level. The preparation method of the ultrapure isopropanol solution and the removal method of trace acetone thereof have the advantages of simple process, high acetone removal rate and low cost, and are suitable for industrialization.)

1. A method for removing trace acetone in an isopropanol solution is characterized in that alkaline solid particles are used as an adsorbent to remove acetone in the isopropanol solution, and the main components of the adsorbent comprise activated alumina, sodium bisulfite, potassium permanganate, an adhesive and a foaming agent.

2. The method for removing the trace acetone in the isopropanol solution as claimed in claim 1, wherein the isopropanol solution passes through an adsorption device at normal temperature and pressure, and the contact time is 5-15 seconds.

3. The method for removing the trace acetone in the isopropanol solution according to claim 1, wherein the mass parts of the main components of the adsorbent are 50-70 parts of activated alumina, 15-25 parts of sodium bisulfite, 5-12 parts of potassium permanganate, 3-4 parts of an adhesive and 1-2 parts of a foaming agent.

4. The method for removing trace acetone in an isopropanol solution as claimed in claim 3, wherein the adsorbent is mixed according to a ratio, and the mixture is baked into granules at 100 ℃ and 150 ℃ and then added into an adsorption device.

5. The method of claim 1, wherein the removal rate of acetone is greater than 98% and the acetone content is less than 2 PPM.

6. A preparation method of an ultrapure isopropanol solution is characterized in that a preparation system of the ultrapure isopropanol solution is used, and the preparation method comprises the following specific steps:

s1, removing acetone: using the acetone removal method according to any one of claims 1 to 5 to obtain an isopropanol solution after acetone removal;

s2, ion removal: the isopropanol solution after the acetone removal enters an ion adsorption device to obtain the isopropanol solution after the metal ions are removed;

s3, rectification: and the isopropanol solution after the metal ions are removed enters a rectifying tower for rectification to obtain an isopropanol solution product meeting the semiconductor chip level.

7. The method for preparing the ultrapure isopropanol solution according to claim 6, wherein the system for preparing the ultrapure isopropanol solution comprises a raw material tank, a delivery pump, an acetone adsorption device, an ion adsorption device, a rectification column, a heat exchanger and a finished product tank which are sequentially communicated, and the rectified isopropanol solution product is finally passed through the heat exchanger to store the finished product in the finished product tank.

8. The method for removing trace acetone in isopropanol solution as claimed in claim 7, wherein the acetone adsorption device is an adsorption column or a tower, and the mode is fixed horizontal or vertical.

9. The method according to claim 7, wherein the adsorption resin in the ion adsorption unit is a reactive ion removal resin.

Technical Field

The invention relates to the field of electronics, in particular to a preparation method of an ultrapure isopropanol solution and a method for removing trace acetone in the isopropanol solution.

Background

The electronic chip industry has increasingly stringent controls on the various impurities, particularly harmful impurities, using large amounts of ultra-pure isopropanol as a necessary cleaning between processing steps. In the quality of the ultrapure isopropanol, one of the key indexes is the content of acetone in the product, which determines the grade of the product and generally requires to be controlled in the range of 1-3 PPM. In practical purification manufacturing processes, it is difficult to control acetone within this desired range.

Disclosure of Invention

The invention mainly solves the technical problem of providing a preparation method of an ultrapure isopropanol solution and a method for removing trace acetone thereof, and the acetone removal rate is high.

In order to solve the technical problems, the invention adopts a technical scheme that: the method for removing the trace acetone in the isopropanol solution is characterized in that alkaline solid particles are used as an adsorbent to remove the acetone in the isopropanol solution, and the main components of the adsorbent comprise activated alumina, sodium bisulfite, potassium permanganate, an adhesive and a foaming agent.

In a preferred embodiment of the invention, the isopropanol solution passes through an adsorption device at normal temperature and pressure, and the contact time is 5-15 seconds.

In a preferred embodiment of the invention, the main components of the adsorbent comprise, by mass, 50-70 parts of activated alumina, 15-25 parts of sodium bisulfite, 5-12 parts of potassium permanganate, 3-4 parts of an adhesive and 1-2 parts of a foaming agent.

In a preferred embodiment of the invention, after the adsorbents are mixed according to the mixture ratio, the mixture is baked into granules at the temperature of 100 ℃ and 150 ℃, and then the granules are added into an adsorption device.

In a preferred embodiment of the present invention, the acetone removal rate is greater than 98% and the acetone content is less than 2 PPM.

In order to solve the technical problem, the invention adopts another technical scheme that: the preparation method of the ultrapure isopropanol solution comprises the following specific steps:

s1, removing acetone: the isopropanol solution after the acetone is removed is obtained by adopting the acetone removal method;

s2, ion removal: the isopropanol solution after the acetone removal enters an ion adsorption tank to obtain the isopropanol solution after the metal ions are removed;

s3, rectification: and the isopropanol solution after the metal ions are removed enters a rectifying tower for rectification to obtain an isopropanol solution product meeting the semiconductor chip level.

In a preferred embodiment of the invention, the system for preparing the ultrapure isopropanol solution comprises a raw material tank, a delivery pump, an acetone adsorption device, an ion adsorption device, a rectifying tower, a heat exchanger and a finished product tank which are sequentially communicated, wherein the rectified isopropanol solution product is finally stored into the finished product tank through the heat exchanger.

In a preferred embodiment of the present invention, the acetone adsorption device is an adsorption column or a tower, and the mode is a fixed horizontal type or a vertical type.

In a preferred embodiment of the present invention, the adsorption resin in the ion adsorption device is a reactive ion removal resin.

The invention has the beneficial effects that: the preparation method of the ultrapure isopropanol solution and the removal method of trace acetone thereof have the advantages of simple process, high acetone removal rate and low cost, and are suitable for industrialization.

Drawings

FIG. 1 is a schematic diagram of a preferred embodiment of a system for preparing an ultrapure isopropanol solution of the present invention;

the parts in the drawings are numbered as follows: 1-raw material tank, 2-transfer pump, 3-acetone adsorption device, 4-ion adsorption device, 5-rectifying tower, 6-heat exchanger and 7-finished product tank.

Detailed Description

The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.

Referring to fig. 1, an embodiment of the present invention includes:

a system for preparing an ultrapure isopropanol solution comprising: a raw material tank 1, a delivery pump 2, an acetone adsorption device 3, an ion adsorption device 4, a rectifying tower 5, a heat exchanger 6 and a finished product tank 7 which are sequentially communicated through pipelines. The conveying pump 2 conveys the raw material of the isopropanol solution from the raw material tank 1 to the acetone adsorption device 3, then conveys the raw material to the ion adsorption device 4, then enters the rectifying tower 5 for rectification, and the rectified and gasified isopropanol solution is liquefied by the heat exchanger 6 and finally enters the finished product tank 7 for storage. The adsorbent of the acetone adsorption device 3 adopts alkaline solid particles. The adsorption resin in the ion adsorption device is a reactive ion removal resin. The acetone adsorption device is an adsorption column or a tower, and the acetone adsorption device is fixed horizontal or vertical.

The method for removing the trace acetone in the isopropanol solution adopts alkaline solid particles as an adsorbent to remove the acetone in the isopropanol solution, and the main components of the adsorbent comprise active alumina, sodium bisulfite, potassium permanganate, an adhesive and a foaming agent. The adsorbent comprises the following main components, by mass, 50-70 parts of activated alumina, 15-25 parts of sodium bisulfite, 5-12 parts of potassium permanganate, 3-4 parts of an adhesive and 1-2 parts of a foaming agent. After the adsorbents are mixed according to the proportion, the mixture is baked to be granulated at the temperature of 100 ℃ and 150 ℃, and then the mixture is added into an adsorption device. The isopropanol solution passes through an adsorption device at normal temperature and normal pressure, and the contact time is 5-15 seconds. The acetone removal rate is more than 98%. The method for removing trace acetone in the isopropanol solution of the invention finds a scientific and simple material and process through a large number of scientific experiments: an efficient adsorbent is developed by utilizing the chemical property of acetone, so that the quality of the isopropanol meets the standard requirement.

The preparation method of the ultrapure isopropanol solution adopts a preparation system of the ultrapure isopropanol solution shown in figure 1, and comprises the following specific steps: allowing the raw material of the isopropanol solution to pass through the acetone adsorption device 3 at normal temperature and normal pressure, wherein the contact time is 5-15 seconds, so as to obtain the isopropanol solution after acetone removal; the removal rate of the acetone is more than 98 percent, and the content of the acetone is less than 2 PPM. In order to effectively prevent the pollution of ions in the product, the isopropanol solution after the acetone removal enters the ion adsorption tank 4 to obtain the isopropanol solution after the metal ions are removed; and the isopropanol solution after the metal ions are removed enters a rectifying tower 5 for rectification to obtain an isopropanol solution product meeting the semiconductor chip level, and finally the isopropanol solution product passes through a heat exchanger 6 and is stored into a finished product tank 7. The preparation method of the ultrapure isopropanol solution has the advantages of simple whole process, short flow time, suitability for industrialization, high acetone removal rate and low cost.

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 of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.