Laboratory high-purity solvent preparation device and method for preparing high-purity solvent

Abstract

The present invention discloses a laboratory high-purity solvent preparation device, which is characterized in that it includes: a solvent tank; a pneumatic pump: it is connected to a first inlet and outlet liquid pipeline on which a filter module is provided and a second inlet and outlet liquid pipeline for extending into the solvent tank at the end, the first inlet and outlet liquid pipeline is provided with a sampling port, and the second inlet and outlet liquid pipeline is provided with nitrogen protection; the filter module includes a particle filter and a metal adsorption device connected to the particle filter through a pipeline, which is a columnar pipeline provided with an adsorbent. The preparation method includes the steps of: 1) raw material loading: preparing a solvent tank, connecting the first inlet pipeline and the second inlet pipeline, and opening a nitrogen bottle; 2) filtration and purification: connecting the particle filter to the columnar pipeline, under nitrogen protection, turning on the pneumatic pump, and the purified reagent passes through the particle filter and the columnar pipeline in succession. After circulating for 2-7 days, it reaches the use standard. It is easy to operate and can purify ordinary commercially available analytical grade solvents to electronic grade.

Description

Technical Field

[0001] The invention relates to a high-purity solvent preparation device for laboratory use and a method for preparing the high-purity solvent. Background Art

[0002] High-purity specialty solvents, a niche segment of the chemical reagent industry, are fundamental and functional materials widely used in industries such as environmental testing, bioengineering, life sciences, pharmaceuticals, food, petrochemicals, scientific research, and electronics, and are a crucial pillar of social development. Within the high-purity specialty solvent sector, varying impurity levels, such as trace metals, water, and organic matter, are required for different applications. Consequently, different product grades exist. The electronics, solar energy, and military sectors primarily utilize electronic-grade, ultra-clean, high-purity reagents, which place high demands on solvent purity.

[0003] Among the electronic-grade solvents used in the integrated circuit industry, mid- and low-end products have been domestically produced, but the high-end products are still monopolized by foreign countries. Taking advanced photoresists as an example, the high-purity solvents used in the high-end integrated circuit industry require a water content of <0.5%, a metal ion content of <1ppb, and a particle size (greater than 0.15 microns) of <10 particles / mL, to ensure that the chips will not be contaminated by the cleaning solvents during the manufacturing process, which would affect the performance of the circuit. In the manufacture of integrated circuits, the supply and use of high-end electronic-grade reagents can be met through a systematic centralized liquid supply system. However, setting up such a system in the laboratory is often extremely costly and difficult to achieve. Currently, the country is vigorously supporting the development of high-end electronic material products such as photoresists. During the development of photoresists, how to manufacture simple, practical, and low-cost high-purity solvent preparation equipment to meet the production requirements of photoresists is a major challenge facing the industry. Currently, chip factories use high-purity solvents imported from countries like Japan, which don't have particle size issues. However, when it comes to photoresist formulation development, the primary focus of production details is the solvent's particle size. However, the particle size of high-purity solvents sold domestically cannot meet the requirements for high-end photoresist formulation development. Specifically, the packaging and quality of domestically produced solvents, as well as their particle size and impurities in high-end applications, are still not up to par with foreign standards. Currently, there is no dedicated preparation equipment for high-purity solvents used in laboratories for both chip production and photoresist formulation development. Laboratories typically use relatively small amounts of solvent and limited space. Therefore, developing more practical, simpler, and portable high-purity solvent preparation equipment, including methods for preparing high-purity solvents in laboratories to meet the demand for high-end electronic-grade reagents in photoresist product development, is an industry challenge that urgently needs to be addressed. Summary of the Invention

[0004] Based on the above-mentioned defects of the prior art, the present invention proposes a high-purity solvent preparation device for laboratory use, which can purify ordinary commercially available analytical-grade solvents to electronic grade, and is simple, practical and low-cost.

[0005] The technical solution of the present invention is achieved as follows:

[0006] The present invention provides a laboratory high-purity solvent preparation device, comprising:

[0007] A solvent tank for storing the solvent to be purified;

[0008] A pneumatic pump for driving solvent circulation: the pneumatic pump is connected to a first inlet and outlet liquid pipeline with a filter module provided thereon and a second inlet and outlet liquid pipeline with the end extending into the solvent tank, the first inlet and outlet liquid pipeline is provided with a sampling port, and the second inlet and outlet liquid pipeline is provided with nitrogen protection; the filter module includes a particle filter for filtering particles and a metal adsorption device connected to the particle filter through a pipeline, and the metal adsorption device is a columnar pipeline provided with an adsorbent.

[0009] As a further improvement of the present invention, the solvent to be purified is a common AR-grade reagent.

[0010] As a further improvement of the present invention, the nitrogen protection outputs nitrogen through a nitrogen bottle pipeline, one path of which is connected to the nitrogen protection port on the second liquid inlet and outlet pipeline, and the other path is connected to the tail gas pipe.

[0011] As a further improvement of the present invention, the solvent to be purified passes through a particle filter and a columnar pipe in sequence, wherein the diameter of the columnar pipe is 10-15 cm;

[0012] The adsorbent is a combination of a strong acid cationic resin mainly composed of sulfonic acid groups or a weak acid cationic resin mainly composed of carboxyl groups and activated carbon:

[0013] That is, a strong acid cationic resin mainly composed of sulfonic acid groups or a weak acid cationic resin mainly composed of carboxyl groups is successively filled in, and then activated carbon is filled in, with an interval of more than 6 layers;

[0014] The strong acid cationic resin or the weak acid cationic resin mainly composed of carboxyl groups and the activated carbon are arranged in a mass ratio of (2-5):1.

[0015] As a further improvement of the present invention, the accuracy of the particle filter is 10nm-100nm.

[0016] As a further improvement of the present invention, it also includes a mobile trolley that functions as a carrying device.

[0017] The present invention also provides a method for preparing a high-purity solvent using a high-purity solvent preparation device for laboratory use that is easy to operate, comprising the following steps:

[0018] 1) Raw material loading: Prepare the solvent tank for the solvent to be purified, connect the first liquid inlet pipeline and the second liquid inlet pipeline, and open the nitrogen bottle to implement nitrogen protection;

[0019] 2) Filtration and purification: After connecting multiple particle filters to a columnar pipe equipped with an adsorbent, start the pneumatic pump under nitrogen protection. After the purified reagent passes through the particle filter and the columnar pipe in succession and circulates for 2-7 days, it reaches the use standard.

[0020] As a further improvement of the present invention, the solvent to be purified is a common AR-grade reagent; the solvent tank, particle filter, columnar pipe and pneumatic pump are all arranged on a mobile cart.

[0021] As a further improvement of the present invention, the adsorbent is a combination of a strong acid cationic resin mainly containing sulfonic acid groups or a weak acid cationic resin mainly containing carboxyl groups and activated carbon:

[0022] That is, acidic resin, strong acidic cationic resin or weak acidic cationic resin mainly composed of carboxyl groups are filled in sequence, and then activated carbon is filled in, and the layers are arranged at intervals for a total of more than 6 layers.

[0023] As a further improvement of the present invention, the mass ratio of the strong acid cationic resin or the weak acid cationic resin mainly composed of carboxyl groups to the activated carbon is (2-5):1.

[0024] The present invention provides a laboratory-use high-purity solvent preparation device that is compact, simple, and practical, allowing for convenient laboratory use while ensuring the safety of particles and metals. The system also has the ability to produce high-purity electronic-grade solvents. Users can purchase domestically supplied common AR-grade reagents, install them in the system, and purify them to obtain electronic-grade solvents, eliminating the need to purchase imported high-purity reagents. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a schematic diagram of the structure of a high-purity solvent preparation device for laboratory use in an embodiment. DETAILED DESCRIPTION

[0026] The laboratory high-purity solvent preparation device of this embodiment is shown in FIG. Figure 1 Shown, including:

[0027] A solvent tank for storing the solvent to be purified;

[0028] A pneumatic pump for driving solvent circulation: the pneumatic pump is connected to a first inlet and outlet liquid pipeline with a filter module provided thereon and a second inlet and outlet liquid pipeline with the end extending into the solvent tank, the first inlet and outlet liquid pipeline is provided with a sampling port, and the second inlet and outlet liquid pipeline is provided with nitrogen protection; the filter module includes a particle filter for filtering particles and a metal adsorption device connected to the particle filter through a pipeline, and the metal adsorption device is a columnar pipeline provided with an adsorbent.

[0029] The solvent to be purified is a common AR grade reagent.

[0030] The nitrogen protection outputs nitrogen through a nitrogen bottle pipeline, one path of which is connected to the nitrogen protection port on the second liquid inlet and outlet pipeline, and the other path is connected to the tail gas pipe.

[0031] The solvent to be purified passes through a particle filter and a columnar pipe in sequence, wherein the diameter of the columnar pipe is 10-15 cm;

[0032] The adsorbent is a combination of a strong acid cationic resin mainly composed of sulfonic acid groups or a weak acid cationic resin mainly composed of carboxyl groups and activated carbon:

[0033] That is, a strong acid cationic resin mainly composed of sulfonic acid groups or a weak acid cationic resin mainly composed of carboxyl groups is successively filled in, and then activated carbon is filled in, with an interval of more than 6 layers;

[0034] The strong acid cationic resin or the weak acid cationic resin mainly composed of carboxyl groups and the activated carbon are arranged in a mass ratio of (2-5):1.

[0035] The particle filter has a precision of 10 nm to 100 nm.

[0036] It also includes a mobile trolley that serves as a carrier.

[0037] A method for preparing a high-purity solvent using a high-purity solvent preparation device for a laboratory that is easy to operate comprises the following steps:

[0038] 1) Raw material loading: Prepare the solvent tank for the solvent to be purified, connect the first liquid inlet pipeline and the second liquid inlet pipeline, and open the nitrogen bottle to implement nitrogen protection;

[0039] 2) Filtration and purification: After connecting multiple particle filters to a columnar pipe equipped with an adsorbent, start the pneumatic pump under nitrogen protection. After the purified reagent passes through the particle filter and the columnar pipe in succession and circulates for 2-7 days, it reaches the use standard.

[0040] The solvent to be purified is a common AR-grade reagent; the solvent tank, particle filter, columnar pipe and pneumatic pump are all arranged on a mobile cart.

[0041] The adsorbent is a combination of a strong acid cationic resin mainly composed of sulfonic acid groups or a weak acid cationic resin mainly composed of carboxyl groups and activated carbon:

[0042] That is, acidic resin, strong acidic cationic resin or weak acidic cationic resin mainly composed of carboxyl groups are filled in sequence, and then activated carbon is filled in, and the layers are arranged at intervals for a total of more than 6 layers.

[0043] The mass ratio of the strong acid cationic resin or the weak acid cationic resin mainly composed of carboxyl groups to the activated carbon is (2-5):1.

[0044] The mobile cart is used to place equipment such as solvent tanks, pneumatic pumps, and filter modules. As a high-purity solvent preparation platform, the mobile cart is convenient and portable, saving laboratory space.

[0045] The pneumatic pump drives the solvent circulation, and the use of a pneumatic pump avoids the use of explosion-proof electrical equipment, thereby increasing safety.

[0046] The filtration module is a filtration and purification module, and its functions include particle filtration and metal impurity adsorption. In terms of particles, the goal can be achieved by purchasing mature domestic particle filters. In terms of metal impurities, the metal adsorbent of the present invention is used to purify commercially available solvents. The metal adsorbent uses a strong acid cationic resin mainly composed of sulfonic acid groups or a weak acid cationic resin mainly composed of carboxyl groups, and is purified in a combination of acidic resin and activated carbon, and can be recycled through conventional activation treatment. The specific combination is a layer of acidic resin, a layer of activated carbon, and a cylindrical pipe with a diameter of 10-15cm. Acidic resin is filled in 3cm high, and then activated carbon is filled in 3cm high, with a total of 6 layers. This treatment method makes the purification effect better. The acidic resin and activated carbon can also be mixed and filled into the pipe of the purification device. Among them, the acidic resin is used to adsorb large metal ions, and the activated carbon adsorbs a small amount of organic impurities and metal impurities.

[0047] The first inlet and outlet liquid pipeline and the second inlet and outlet liquid pipeline are used as solvent circulation pipelines, fixed clean pipelines, and provide clean pipelines for liquid circulation.

[0048] The function of nitrogen protection is to provide nitrogen protection to the filtration system, which can keep the moisture content of the solvent from increasing.

[0049] Sampling port, solvent taking port.

[0050] Experimental Verification: Gold impurities were tested using ICP-MS, and particles were tested using a particle analyzer. Operational Procedure: A purification system was constructed, and 0.1 micron and 50 nanometer particle filters were installed in the filtration module. During the metal purification module installation, a mixture of a strongly acidic cationic resin or a weakly acidic cationic resin primarily based on carboxyl groups and activated carbon was placed in a columnar tube at a mass ratio of (2-5):1. The experimental results are shown in Table 1 below:

[0051] Table 1 Comparison of particle size and metal impurities under different conditions

[0052] project Particle size (greater than 0.1 micron) Gold and Miscellaneous This program <10 cells / mL <5ppb Large centralized supply <10 cells / mL <5ppb Laboratory conditions >500 cells / mL >300ppb

[0053] During the development of high-purity electronic materials, such as photoresists, if the particle size or metallic impurity content of the reagents used is too high, the silicon wafer surface will contain a large number of particles after the photoresist is applied, resulting in increased defects in the pattern during photolithography and affecting analytical results. The above table shows that the laboratory-use high-purity solvent preparation device and method of preparing high-purity solvents of this embodiment can purify common commercially available analytical-grade solvents to electronic grade while being simple and easy to use, allowing for flexible use in the laboratory and having high practicality.

[0054] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field fall within the scope of protection of the present invention. The above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A high-purity solvent preparation device for laboratory use, characterized in that: include: A solvent tank for storing the solvent to be purified; A pneumatic pump for driving solvent circulation: the pneumatic pump is connected to a first inlet and outlet liquid pipeline on which a filter module is installed and a second inlet and outlet liquid pipeline whose end extends into the solvent tank, the first inlet and outlet liquid pipeline is provided with a sampling port, and the second inlet and outlet liquid pipeline is provided with nitrogen protection; the filter module includes a particle filter for filtering particles and a metal adsorption device connected to the particle filter via a pipeline, the metal adsorption device being a columnar pipe provided with an adsorbent; The solvent to be purified is a common AR grade reagent; The solvent to be purified passes through a particle filter and a columnar pipe in sequence, wherein the diameter of the columnar pipe is 10-15 cm; The adsorbent is a combination of a strong acid cationic resin mainly composed of sulfonic acid groups or a weak acid cationic resin mainly composed of carboxyl groups and activated carbon: That is, a strong acid cationic resin mainly composed of sulfonic acid groups or a weak acid cationic resin mainly composed of carboxyl groups is successively filled in, and then activated carbon is filled in, with an interval of more than 6 layers; The strong acid cationic resin or the weak acid cationic resin mainly composed of carboxyl groups and the activated carbon are arranged in a mass ratio of (2-5):1; The nitrogen protection outputs nitrogen through the nitrogen bottle pipeline, one of which is connected to the nitrogen protection port on the second liquid inlet and outlet pipeline, and the other is connected to the tail gas pipe; The particle filter has a precision of 10 nm to 100 nm.

2. The laboratory high-purity solvent preparation device according to claim 1, characterized in that: It also includes a mobile trolley that serves as a carrier.

3. A method for preparing a high-purity solvent using the laboratory high-purity solvent preparation device according to any one of claims 1-2, characterized in that The following steps are involved: 1) Raw material loading: Prepare the solvent tank for the solvent to be purified, connect the first liquid inlet pipeline and the second liquid inlet pipeline, and open the nitrogen bottle to implement nitrogen protection; 2) Filtration and purification: After connecting multiple particle filters to a columnar pipe equipped with an adsorbent, start the pneumatic pump under nitrogen protection. After the purified reagent passes through the particle filter and the columnar pipe in succession and circulates for 2-7 days, it reaches the use standard.

4. The method according to claim 3, characterized in that The solvent to be purified is a common AR-grade reagent; the solvent tank, particle filter, columnar pipe and pneumatic pump are all arranged on a mobile cart.

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