A high-concentration ozone preparation device and a preparation method thereof

Abstract

This invention discloses a high-concentration ozone preparation device, comprising the following components: an ozone generator (1), an oxygen blower (6); a first adsorption tower (2) and a second adsorption tower (3); a purification tower (4), an oxygen buffer tank (5), an ozone tank (7), a vacuum buffer tank (8), and a vacuum pump (9). This invention also discloses a method for preparing high-concentration ozone.

Description

Technical Field

[0001] This invention belongs to the field of chemical engineering, and specifically relates to a high-concentration ozone preparation device and preparation method. Background Technology

[0002] Ozone, due to its strong oxidizing properties, is widely used in water treatment, medical sterilization, and industrial oxidation. Currently, industrial ozone is mainly produced through a discharge reaction of high-purity oxygen; however, due to limitations in reaction efficiency, the concentration of the mixed gas output by ozone generators is typically below 150 mg / L. However, applications such as high-salinity wastewater treatment and fine chemical production require higher ozone concentrations, which current technologies cannot directly meet.

[0003] To increase ozone concentration, adsorption concentration methods are widely used. For example, CN102989262B proposes using a dual-adsorption cylinder pressure equalization technology to reduce the initial desorption pressure; however, it is limited by passive pressure equalization and single vacuum suction, resulting in high dead zone residue. CN113304582B designs a multi-tower pressure swing adsorption process to buffer pressure fluctuations through a pressure equalization step; however, the system is complex, requiring at least four towers and a maximum concentration of 600 mg / L, while failing to solve the oxygen recovery problem. CN107754555B develops a two-tower adsorption-desorption cycle to achieve oxygen reuse; however, it requires external air or nitrogen flushing and regeneration, directly reducing the final ozone concentration.

[0004] Existing technologies suffer from three major drawbacks: 1. Severe waste of oxygen resources. The oxygen conversion rate of ozone generators is only about 10%, with 90% of the oxygen emitted with the exhaust gas; since oxygen production costs account for more than 60% of the total production cost, the waste is significant and costs are high. 2. Difficulty in balancing concentration and efficiency. Multi-tower systems, such as 4-10 towers, can increase concentration, but the equipment is complex and energy-intensive; dual-tower systems rely on external gas sources for regeneration, limiting the purity of oxygen circulation; and adsorbent regeneration is incomplete. 3. Traditional equalization or rinsing steps cannot remove residual ozone in the adsorbent dead zone, and insufficient vacuum desorption pressure (typically -90 kPa) limits the final concentration.

[0005] Therefore, there is an urgent need to develop a high-concentration ozone preparation technology with a simplified structure, closed-loop oxygen circulation, and deep desorption and regeneration, so as to break through the concentration bottleneck and maximize resource utilization.

[0006] This invention is proposed for this purpose. Summary of the Invention

[0007] This invention discloses a high-concentration ozone preparation device, which can be used to prepare ozone with a concentration greater than 600 mg / L.

[0008] The technical solution of the present invention is as follows:

[0009] The first invention discloses a high-concentration ozone preparation device, comprising the following components:

[0010] Ozone generator 1, whose inlet is connected to the outlet of oxygen blower 6;

[0011] The first adsorption tower 2 and the second adsorption tower 3 are arranged in parallel; the outlet of the ozone generator 1 is connected to the top or bottom of the first adsorption tower 2 and the second adsorption tower 3 respectively through a switching valve group, and is also connected to the bottom inlet of the first adsorption tower 2 and the second adsorption tower 3 respectively.

[0012] The purification tower 4 has its bottom inlet connected to the top outlet of the first adsorption tower 2 and the second adsorption tower 3, and its top outlet connected to the inlet of the oxygen blower 6 via the oxygen buffer tank 5.

[0013] The bottoms of the first adsorption tower 2 and the second adsorption tower 3 are connected to the ozone tank 7 via a switching valve group; the outlet of the ozone tank 7 is also connected to the vacuum pump 9 via a vacuum buffer tank 8.

[0014] Preferably, the first adsorption tower 2 and the second adsorption tower 3 are filled with ozone selective adsorbent; the purification tower 4 is filled with ozone decomposition catalyst.

[0015] Preferably, the ozone selective adsorbent is a molecular sieve adsorbent; the ozone decomposition catalyst is a manganese-copper composite oxide catalyst; wherein the applicant has separately applied for patent protection for the molecular sieve adsorbent and its preparation method.

[0016] A second aspect of this invention discloses a method for preparing high-concentration ozone, using any of the apparatus described above, comprising the following steps:

[0017] (A) The oxygen blower 6 introduces oxygen into the ozone generator 1 to generate a low-concentration ozone and oxygen mixture with an ozone concentration of less than 150 mg / L as the raw material gas; (B) The raw material gas is alternately introduced into the first adsorption tower 2 and the second adsorption tower 3 for alternating pressure swing adsorption.

[0018] (C) The adsorbed exhaust gas enters the purification tower 4. The residual ozone in the exhaust gas is catalytically decomposed by the ozone decomposition catalyst in the purification tower 4 to generate oxygen. After being pressurized by the oxygen buffer tank 5 and the oxygen blower 6, it is returned to the ozone generator 1 for recycling. (D) The first adsorption tower 2 and the second adsorption tower 3 are regenerated in sequence through the following steps: (D1) Countercurrent purging: When the pressure of the first adsorption tower 2 or the second adsorption tower 3 drops to atmospheric pressure, the direction of the raw material gas inlet is switched so that the raw material gas enters from the top of the tower and the residual ozone carried is discharged from the bottom of the tower. (D2) Deep vacuum desorption: Desorption is performed using a vacuum pump 9 at a pressure of -0.09 ~ -0.095 MPa.

[0019] The countercurrent purge gas and vacuum desorption gas are combined and stored in ozone tank 7, which outputs high-concentration ozone with an ozone concentration >600 mg / L.

[0020] Preferably, the first adsorption tower 2 and the second adsorption tower 3 alternately perform pressure swing adsorption in a four-step cycle, with each cycle including:

[0021] Step 1: Adsorption in the first adsorption tower 2 and vacuum regeneration in the second adsorption tower 3;

[0022] In the first adsorption tower 2, low-concentration ozone raw gas enters from the bottom of the tower, and exhaust gas is discharged from the top of the tower into the purification tower 4.

[0023] In the second adsorption tower 3, the vacuum pump 9 draws gas from the bottom of the tower for desorption, and the gas is input into the ozone tank 7;

[0024] Step 2: First adsorption tower 2 is countercurrently purged and second adsorption tower 3 is pressurized and ready for use;

[0025] In the first adsorption tower 2, when the pressure drops to atmospheric pressure, the raw material gas is switched to enter from the top of the tower, and the purging gas is discharged from the bottom of the tower into the ozone tank 7.

[0026] The second adsorption tower 3 has completed vacuum regeneration and is now under pressure for use.

[0027] Step 3: Vacuum regeneration of the first adsorption tower 2 and adsorption in the second adsorption tower 3;

[0028] In the first adsorption tower 2, the vacuum pump 9 draws gas from the bottom of the tower for desorption, and the gas is input into the ozone tank 7;

[0029] The second adsorption tower 3 receives raw gas from the bottom and exhaust gas from the top into the purification tower 4; Step 4: The first adsorption tower 2 is pressurized and ready for use, while the second adsorption tower 3 is purged countercurrently.

[0030] First adsorption tower 2, vacuum regeneration completed, pressure maintained and ready for use;

[0031] In the second adsorption tower 3, when the pressure drops to atmospheric pressure, the raw material gas is switched to enter from the top of the tower, and the purging gas is discharged from the bottom of the tower into the ozone tank 7.

[0032] The beneficial effects of this invention are:

[0033] 1. This invention utilizes a high-concentration ozone preparation device, employing a combined regeneration method of "countercurrent purging + deep vacuum desorption," achieving a final output ozone concentration stably exceeding 600 mg / L. This significantly surpasses the concentration levels of existing dual-tower systems, which are generally below 300 mg / L. It can meet the needs of high-concentration ozone applications such as high-salt wastewater treatment and fine chemical production.

[0034] 2. The high-concentration ozone preparation device of the present invention uses only two towers for alternating adsorption and regeneration, achieving continuous and efficient operation through a four-step cyclical process. This avoids the complex pressure equalization steps and high equipment investment of existing multi-tower systems such as 4-10 towers; it reduces system complexity and floor space while maintaining high ozone concentration output and high recovery efficiency, thus combining economic efficiency and practicality.

[0035] 3. The preparation method of this invention includes a "countercurrent purging" step before vacuum desorption, using the raw material gas to purge residual ozone from the top of the tower, reducing dead zone accumulation. Subsequent deep vacuum further enhances the desorption effect. The dual regeneration mechanism ensures complete regeneration of the ozone selective adsorbent, extending its service life and improving system stability. The ozone selective adsorbent is a molecular sieve adsorbent, and the applicant has separately applied for patent protection for the molecular sieve adsorbent and its preparation method.

[0036] 4. The high-concentration ozone preparation method of the present invention relies entirely on the internal oxygen and vacuum system of the device for regeneration, without the need for external air or nitrogen purging; it avoids the problem of ozone concentration reduction caused by the introduction of external gas, ensuring the stability of output ozone purity and concentration; it reduces costs and achieves maximum resource utilization. Attached Figure Description

[0037] Figure 1 This is a schematic diagram of the high-concentration ozone preparation device and process of the present invention.

[0038] The attached diagram is labeled as follows: 1-Ozone generator; 2-First adsorption tower; 3-Second adsorption tower; 4-Purification tower; 5-Oxygen buffer tank; 6-Oxygen blower; 7-Ozone tank; 8-Vacuum buffer tank; 9-Vacuum pump. Detailed Implementation

[0039] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention. Furthermore, the technical features involved in the various embodiments of this invention described below can be combined with each other as long as they do not conflict with each other.

[0040] In the description of this invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0041] Furthermore, the terms “first”, “second”, etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated.

[0042] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "joining," "fixing," "adhesion," etc., should be interpreted broadly. For example, they can refer to a connection, a detachable connection, or an integral part. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0043] In this specification, the illustrative expressions of the terms used above should not be construed as necessarily referring to the same embodiments or examples. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, those skilled in the art can combine and integrate the different embodiments or examples described in this specification.

[0044] like Figure 1 The high-concentration ozone preparation device shown includes the following components:

[0045] Ozone generator 1, whose inlet is connected to the outlet of oxygen blower 6;

[0046] The first adsorption tower 2 and the second adsorption tower 3 are arranged in parallel; the outlet of the ozone generator 1 is connected to the top or bottom of the first adsorption tower 2 and the second adsorption tower 3 respectively through a switching valve group, and is also connected to the bottom inlet of the first adsorption tower 2 and the second adsorption tower 3 respectively.

[0047] The purification tower 4 has its bottom inlet connected to the top outlet of the first adsorption tower 2 and the second adsorption tower 3, and its top outlet connected to the inlet of the oxygen blower 6 via the oxygen buffer tank 5.

[0048] The bottoms of the first adsorption tower 2 and the second adsorption tower 3 are connected to the ozone tank 7 via a switching valve group; the outlet of the ozone tank 7 is also connected to the vacuum pump 9 via a vacuum buffer tank 8.

[0049] The first adsorption tower 2 and the second adsorption tower 3 are filled with ozone selective adsorbents; the purification tower 4 is filled with ozone decomposition catalysts.

[0050] The ozone selective adsorbent is a molecular sieve adsorbent; the ozone decomposition catalyst is a manganese-copper composite oxide catalyst; the applicant has separately applied for patent protection for the molecular sieve adsorbent and its preparation method, see patent CN2026104261357. The molecular sieve adsorbent of this invention uses the molecular sieve adsorbent of Example 1 of patent CN2026104261357.

[0051] The method for preparing high-concentration ozone using the above-mentioned high-concentration ozone preparation device includes the following steps:

[0052] (A) The oxygen blower 6 introduces oxygen into the ozone generator 1 to generate a low-concentration ozone and oxygen mixture with an ozone concentration of less than 150 mg / L as the raw material gas; (B) The raw material gas is alternately introduced into the first adsorption tower 2 and the second adsorption tower 3 for alternating pressure swing adsorption.

[0053] (C) The adsorbed exhaust gas enters the purification tower 4. The residual ozone in the exhaust gas is catalytically decomposed by the ozone decomposition catalyst in the purification tower 4 to generate oxygen. After being pressurized by the oxygen buffer tank 5 and the oxygen blower 6, it is returned to the ozone generator 1 for recycling. (D) The first adsorption tower 2 and the second adsorption tower 3 are regenerated in sequence through the following steps: (D1) Countercurrent purging: When the pressure of the first adsorption tower 2 or the second adsorption tower 3 drops to atmospheric pressure, the direction of the raw material gas inlet is switched so that the raw material gas enters from the top of the tower and the residual ozone carried is discharged from the bottom of the tower. (D2) Deep vacuum desorption: Desorption is performed using a vacuum pump 9 at a pressure of -0.09 ~ -0.095 MPa.

[0054] The countercurrent purge gas and vacuum desorption gas are combined and stored in ozone tank 7, which outputs high-concentration ozone with an ozone concentration >600 mg / L.

[0055] The first adsorption tower 2 and the second adsorption tower 3 alternately operate in a four-step cycle of pressure swing adsorption, with each cycle including:

[0056] Step 1: Adsorption in the first adsorption tower 2 and vacuum regeneration in the second adsorption tower 3;

[0057] In the first adsorption tower 2, low-concentration ozone raw gas enters from the bottom of the tower, and exhaust gas is discharged from the top of the tower into the purification tower 4.

[0058] In the second adsorption tower 3, the vacuum pump 9 draws gas from the bottom of the tower for desorption, and the gas is input into the ozone tank 7;

[0059] Step 2: First adsorption tower 2 is countercurrently purged and second adsorption tower 3 is pressurized and ready for use;

[0060] In the first adsorption tower 2, when the pressure drops to atmospheric pressure, the raw material gas is switched to enter from the top of the tower, and the purging gas is discharged from the bottom of the tower into the ozone tank 7.

[0061] The second adsorption tower 3 has completed vacuum regeneration and is now under pressure for use.

[0062] Step 3: Vacuum regeneration of the first adsorption tower 2 and adsorption in the second adsorption tower 3;

[0063] In the first adsorption tower 2, the vacuum pump 9 draws gas from the bottom of the tower for desorption, and the gas is input into the ozone tank 7;

[0064] The second adsorption tower 3 receives raw gas from the bottom and exhaust gas from the top into the purification tower 4; Step 4: The first adsorption tower 2 is pressurized and ready for use, while the second adsorption tower 3 is purged countercurrently.

[0065] First adsorption tower 2, vacuum regeneration completed, pressure maintained and ready for use;

[0066] In the second adsorption tower 3, when the pressure drops to atmospheric pressure, the raw material gas is switched to enter from the top of the tower, and the purging gas is discharged from the bottom of the tower into the ozone tank 7.

[0067] This invention utilizes a high-concentration ozone preparation device, employing a combined regeneration method of "countercurrent purging + deep vacuum desorption," achieving a stable ozone output concentration exceeding 600 mg / L, with a maximum of 800 mg / L. This significantly surpasses the concentration levels of existing dual-tower systems, which are generally below 300 mg / L (see Absolute Ozone® ATLAS30UHC). It can meet the needs of high-concentration ozone applications such as high-salinity wastewater treatment and fine chemical production. The high-concentration ozone preparation device of this invention uses only two adsorption towers for alternating adsorption and regeneration, achieving continuous and efficient operation through a four-step cyclical process. This avoids the complex pressure equalization steps and high equipment investment of existing multi-tower systems (such as 4-10 towers), reducing system complexity and floor space requirements while maintaining high ozone concentration output and high recovery efficiency, thus combining economic efficiency and practicality. The preparation method of this invention incorporates a "countercurrent purging" step before vacuum desorption, using raw material gas to purge residual ozone from the top of the tower, reducing dead zone accumulation. Subsequent deep vacuum further enhances the desorption effect. This dual regeneration mechanism ensures complete regeneration of the ozone adsorbent, extending its lifespan and improving system stability. The ozone selective adsorbent is a molecular sieve adsorbent; the applicant will separately apply for patent protection for the molecular sieve adsorbent and its preparation method. This invention's high-concentration ozone preparation method relies entirely on the internal oxygen and vacuum system for regeneration, eliminating the need for external air or nitrogen purging. This avoids the problem of ozone concentration decrease caused by the introduction of external gases, ensuring stable output ozone purity and concentration; reducing costs and maximizing resource utilization.

[0068] The above embodiments are not intended to limit the present invention, nor is the present invention limited to the examples described above. Any changes, modifications, additions, or substitutions made by those skilled in the art within the scope of the present invention are also within the protection scope of the present invention.

Claims

1. A high-concentration ozone preparation device, characterized in that, Includes the following components: The ozone generator (1) has its inlet connected to the outlet of the oxygen blower (6); The first adsorption tower (2) and the second adsorption tower (3) are set in parallel; the outlet of the ozone generator (1) is connected to the top or bottom of the first adsorption tower (2) and the second adsorption tower (3) respectively through a switching valve group, and is connected to the bottom inlet of the first adsorption tower (2) and the second adsorption tower (3) respectively. The purification tower (4) has its bottom inlet connected to the top outlet of the first adsorption tower (2) and the second adsorption tower (3), and its top outlet is connected to the inlet of the oxygen blower (6) via the oxygen buffer tank (5). The bottoms of the first adsorption tower (2) and the second adsorption tower (3) are connected to the ozone tank (7) via a switching valve group; the outlet of the ozone tank (7) is also connected to the vacuum pump (9) via a vacuum buffer tank (8).

2. The high-concentration ozone preparation device according to claim 1, characterized in that, The first adsorption tower (2) and the second adsorption tower (3) are filled with ozone selective adsorbent; the purification tower (4) is filled with ozone decomposition catalyst.

3. The high-concentration ozone preparation device according to claim 2, characterized in that, The ozone selective adsorbent is a molecular sieve adsorbent; the ozone decomposition catalyst is a manganese-copper composite oxide catalyst.

4. A method for preparing high-concentration ozone, characterized in that, Using the apparatus according to any one of claims 1-3 includes the following steps: (A) The oxygen blower (6) introduces oxygen into the ozone generator (1) to generate a low-concentration ozone and oxygen mixture with an ozone concentration of less than 150 mg / L as the raw material gas; (B) The raw material gas is alternately introduced into the first adsorption tower (2) and the second adsorption tower (3) for alternating pressure swing adsorption. (C) The adsorbed exhaust gas enters the purification tower (4). The residual ozone in the exhaust gas is catalytically decomposed by the ozone decomposition catalyst in the purification tower (4) to generate oxygen. After being pressurized by the oxygen buffer tank (5) and the oxygen blower (6), it is returned to the ozone generator (1) for recycling. (D) The first adsorption tower (2) and the second adsorption tower (3) are regenerated in sequence through the following steps: (D1) Countercurrent purging: When the pressure of the first adsorption tower (2) or the second adsorption tower (3) drops to atmospheric pressure, the direction of the raw material gas inlet is switched so that the raw material gas enters from the top of the tower and the residual ozone carried is discharged from the bottom of the tower. (D2) Deep vacuum desorption: Desorption is performed by a vacuum pump (9) at a pressure of -0.09 ~ -0.095MPa. The countercurrent purge gas and vacuum desorption gas are combined and stored in the ozone tank (7), which outputs high-concentration ozone with an ozone concentration >600 mg / L.

5. The preparation method according to claim 4, characterized in that, The first adsorption tower (2) and the second adsorption tower (3) alternately operate in a four-step cycle of pressure swing adsorption, each cycle including: Step 1: Adsorption in the first adsorption tower (2) and vacuum regeneration in the second adsorption tower (3); In the first adsorption tower (2), low-concentration ozone raw material gas enters from the bottom of the tower, and exhaust gas is discharged from the top of the tower into the purification tower (4). In the second adsorption tower (3), the vacuum pump (9) draws gas from the bottom of the tower for desorption, and the gas is input into the ozone tank (7); Step 2: First adsorption tower (2) countercurrent purging and second adsorption tower (3) pressure holding for standby; When the pressure in the first adsorption tower (2) drops to atmospheric pressure, the raw material gas is switched to enter from the top of the tower, and the purging gas is discharged from the bottom of the tower into the ozone tank (7). The second adsorption tower (3) has completed vacuum regeneration and is now under pressure for use. Step 3: Vacuum regeneration of the first adsorption tower (2) and adsorption of the second adsorption tower (3); In the first adsorption tower (2), the vacuum pump (9) draws gas from the bottom of the tower for desorption, and the gas is input into the ozone tank (7); In the second adsorption tower (3), the raw gas enters from the bottom of the tower, and the exhaust gas is discharged from the top of the tower into the purification tower (4); Step 4: The first adsorption tower (2) is pressurized and ready for use, and the second adsorption tower (3) is purged in countercurrent. The first adsorption tower (2) has completed vacuum regeneration and is now under pressure for use. When the pressure in the second adsorption tower (3) drops to atmospheric pressure, the raw material gas is switched to enter from the top of the tower, and the purging gas is discharged from the bottom of the tower into the ozone tank (7).

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