Refining method and device of electronic-grade octafluorocyclopentene

Through extraction and rectification methods and multi-stage distillation technology, combined with molecular sieve adsorbents and specific extraction agents, the problem of preparation of high-purity octafluorocyclopentene in the prior art is solved, and the preparation of electronic grade octafluorocyclopentene with high purity and high yield is achieved, which is suitable for semiconductor and microelectronic industries.

CN120289271APending Publication Date: 2025-07-11PERIC SPECIAL GASES CO LTD
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Patent Information

Application Number
CN202510319237.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-18
Publication Date
2025-07-11

AI Technical Summary

Technical Problem

The prior art is difficult to efficiently prepare high-purity electron-grade octafluorocyclopentene, especially in removing impurities such as hydrogen, oxygen, nitrogen, etc., and it is difficult to meet the requirements of the semiconductor and microelectronics industries.

Method used

The extraction and distillation method is adopted to achieve the purification of octafluorocyclopentene through steps such as vaporization, adsorption, extraction and distillation, delight distillation and deweight distillation, combined with molecular sieve adsorbents and specific extraction agents, including the use of molecular sieve adsorbents 13X, HZSM-5, high silicate zeolite and extraction agents such as acetonitrile, DMF, methyl isobutyl ketone, etc., for multi-stage distillation treatment.

Benefits of technology

The purity of electronic grade octafluorocyclopentene is ≥5N and the yield is ≥95%, meeting the high purity requirements of the semiconductor and microelectronics industries, and the process is simple and easy to industrially produce.

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Abstract

The invention discloses a refining method of electronic-grade octafluorocyclopentene. The refining method comprises the following steps: vaporizing an octafluorocyclopentene raw material; adsorbing the vaporized octafluorocyclopentene raw material by using an adsorbent; after adsorption is completed, an adsorbed octafluorocyclopentene raw material is obtained, an extraction agent is added into the adsorbed octafluorocyclopentene raw material for extractive distillation, an octafluorocyclopentene crude fraction is extracted from the tower top in the extractive distillation process, and an extraction agent fraction is extracted from the tower kettle; the obtained octafluorocyclopentene coarse fraction is subjected to light component removal rectification, light components are extracted from the tower top, and an octafluorocyclopentene fraction is extracted from the tower kettle; the prepared octafluorocyclopentene fraction is subjected to heavy component removal rectification, an electronic-grade octafluorocyclopentene product is extracted from the tower top, and heavy components are extracted from the tower kettle. The invention further relates to a refining device of the electronic-grade octafluorocyclopentene. The refining device comprises a vaporizer, an adsorption tower, an extractive distillation tower, a light component removal tower and a heavy component removal tower which are communicated in sequence. The electronic-grade octafluorocyclopentene with the purity of more than or equal to 5N is obtained, and the process is simple.
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Description

Technical Field

[0001] The present invention relates to a method for preparing an electronic-grade gas, and particularly to a refining method and device for electronic-grade octafluorocyclopentene. Background Art

[0002] Octafluorocyclopentene, with the molecular formula C5F8 and alias perfluorocyclopentene, is a toxic, non-flammable colorless liquid under normal temperature and pressure. Its boiling point is 27°C under normal pressure, and the vapor generated by volatilization can cause dizziness in those who come into contact. As an environmentally friendly fluorinated chemical, octafluorocyclopentene does not contain chlorine and bromine elements in its molecule. Its ozone depletion potential DOP is 0, its atmospheric lifetime is 0.98 a, and its global warming potential GWP100 is only 90. It has better environmental performance than currently widely used fluorinated electronic gases such as CF4, C2F6, NF3, c-C4F8, CHF3, and SF6. It can be used to synthesize organic photochromic materials and electronic materials, and can also be used as an etchant and cleaning agent in the semiconductor manufacturing process, having good market prospects.

[0003] Chinese Patent CN201710352004.X proposes a method for preparing octafluorocyclopentene, which includes the following steps: a. In the presence of a fluorination catalyst, 1,4-dichlorohexafluorocyclopentene or / and 1,3-dichlorohexafluorocyclopentene or / and 1,2-dichlorohexafluorocyclopentene undergoes a gas-phase catalytic fluorination reaction with anhydrous hydrogen fluoride to obtain the intermediate 1-chloroheptafluorocyclopentene; b. In the presence of a fluorination catalyst, 1-chloroheptafluorocyclopentene undergoes a gas-phase catalytic fluorination reaction with anhydrous hydrogen fluoride to obtain octafluorocyclopentene. The present invention can achieve zero-pollution production of octafluorocyclopentene. Through the circulation system in the first-step reaction and the second-step reaction, the materials can react completely, achieving the full utilization of the materials, thus greatly reducing pollution and realizing zero-pollution production.

[0004] Chinese Patent CN201880032088.1 proposes a method for manufacturing octafluorocyclopentene, which manufactures octafluorocyclopentene by contacting 1-chloroheptafluorocyclopentene with an alkali metal fluoride, including: a raw material heating step of heating 1-chloroheptafluorocyclopentene to 40°C or higher and 55°C or lower; and a fluorination step of maintaining a suspension containing an aprotic polar solvent and an alkali metal fluoride at 85°C or higher, and supplying the heated 1-chloroheptafluorocyclopentene to the suspension for fluorination to obtain octafluorocyclopentene.

[0005] Chinese Patent CN201711389280.X proposes an industrial production method of octafluorocyclopentene. Using cyclopentene, chlorine gas, and anhydrous potassium fluoride as raw materials, and sulfolane as a solvent, octafluorocyclopentene is produced through stepwise chlorination with programmed temperature increase and high-temperature substitution reaction with potassium fluoride. After separating the product, the residue in the kettle can be reused by vacuum distilling the solvent sulfolane. The production process of the present invention is simple, environmentally friendly, has a high yield, low production cost, and the obtained product has a high purity, which is beneficial for later applications.

[0006] Chinese Patent CN201910809769.0 proposes a purification method for electronic-grade octafluorocyclopentene, including steps such as rectification purification, low-temperature adsorption purification, and pressurized adsorption purification. The present invention uses the gas-phase method to obtain the final product octafluorocyclopentene from easily available raw material cyclopentene. The present invention adopts low-temperature rectification technology, combines low-temperature adsorption technology and pressurized adsorption technology to purify octafluorocyclopentene, and uses modified coconut shell charcoal as a mesoporous low-temperature adsorbent. After further separation and purification by membrane separation, the volume concentration of water impurity in the octafluorocyclopentene product is ≤5 ppm, the volume concentration of oxygen impurity is ≤3.5 ppm, and the volume concentration of nitrogen gas, which is difficult to separate by traditional processes, is <1 ppm, effectively improving the purity of the product and achieving a purity of the octafluorocyclopentene product above 99.999%, meeting the requirements for electronic special gases in the semiconductor and microelectronics industries. Summary of the Invention

[0007] The present invention proposes a refining method and device for electronic-grade octafluorocyclopentene. Using crude octafluorocyclopentene as a raw material, electronic-grade octafluorocyclopentene with a purity ≥5N is refined through extractive distillation.

[0008] The present invention is implemented by adopting the following technical solutions:

[0009] A refining method for electronic-grade octafluorocyclopentene, including the following steps:

[0010] (1) Vaporizing the octafluorocyclopentene raw material;

[0011] (2) Adsorbing the vaporized octafluorocyclopentene raw material with an adsorbent;

[0012] (3) After adsorption, obtaining the adsorbed octafluorocyclopentene raw material, adding an extractant to the adsorbed octafluorocyclopentene raw material for extractive distillation. In the process of extractive distillation, the crude distillate of octafluorocyclopentene is taken out from the top of the tower, and the extractant distillate is taken out from the bottom of the tower;

[0013] (4) Performing light component removal rectification on the crude distillate of octafluorocyclopentene obtained in step (3), taking out the light components from the top of the tower, and taking out the octafluorocyclopentene distillate from the bottom of the tower;

[0014] (5) Distill the octafluorocyclopentene fraction prepared in step (4) to remove heavy components. The electronic-grade octafluorocyclopentene product is taken from the top of the column, and the heavy components are taken from the bottom of the column.

[0015] Preferably, the following steps are further included:

[0016] (6) Send the extractant fraction prepared in step (3) for extractant rectification recovery. Light components are taken from the top of the column, and the extractant is taken from the bottom of the column.

[0017] Preferably, the vaporization operation pressure in step (1) is 0.12 - 0.3 MPa, and the temperature is 30 - 60 °C;

[0018] The adsorption operation pressure in step (2) is 0.12 - 0.3 MPa, and the temperature is 30 - 60 °C;

[0019] The extractive distillation operation pressure in step (3) is 0.12 - 0.2 MPa, and the temperature is 30 - 160 °C;

[0020] The light component removal distillation operation pressure in step (4) is 0.12 - 0.2 MPa, and the temperature is 30 - 160 °C;

[0021] The heavy component removal distillation operation pressure in step (5) is 0.12 - 0.2 MPa, and the temperature is 30 - 160 °C.

[0022] Preferably, the extractant rectification recovery operation pressure in step (6) is 0.12 - 0.2 MPa, and the temperature is 30 - 160 °C.

[0023] Preferably, the adsorbent used in step (2) is one or a mixture of molecular sieve adsorbents 13X, molecular sieve adsorbent HZSM-5, and high-silica zeolite.

[0024] Preferably, the extractant used in the extractive distillation in step (3) is one or a mixture of acetonitrile, DMF, and methyl isobutyl ketone.

[0025] Preferably, the mass ratio of the extractant in step (3) to the octafluorocyclopentene raw material after adsorption is 5 - 15:1.

[0026] Preferably, the purity of the electronic-grade octafluorocyclopentene product taken out is ≥5N, and the yield is ≥95%.

[0027] A refining device for electronic-grade octafluorocyclopentene, comprising a vaporizer, an adsorption tower, an extractive distillation tower, a light component removal tower, and a heavy component removal tower connected in sequence according to the reaction order;

[0028] The top of the vaporizer is connected to the adsorption tower;

[0029] The top of the extractive distillation tower is connected to the light component removal tower, and the bottom of the light component removal tower is connected to the heavy component removal tower.

[0030] Preferably, an extractant recovery column is further included, and the extractant recovery column is connected to the bottom of the extractive distillation column.

[0031] Advantages of the present invention:

[0032] By means of extractive distillation, the present invention obtains electronic-grade octafluorocyclopentene with a purity ≥ 5N. The process of the present invention is simple and is easy to realize the stable industrial production of octafluorocyclopentene.

[0033] The yield of the electronic-grade octafluorocyclopentene product prepared by the present invention is ≥ 95%. Description of the Drawings

[0034] Figure 1 It is a schematic structural diagram of a refining device for electronic-grade octafluorocyclopentene of the present invention.

[0035] E1101: vaporizer, X1101: adsorption column, T1201: extractive distillation column, T1301: light component removal column, T1401: heavy component removal column, T1501: extractant recovery column. Detailed Embodiments

[0036] A refining method for electronic-grade octafluorocyclopentene proposed by the present invention uses crude octafluorocyclopentene as a raw material and obtains electronic-grade octafluorocyclopentene with a purity ≥ 5N by means of extractive distillation. The process of the present invention is simple and is easy to realize the stable industrial production of octafluorocyclopentene.

[0037] The detailed embodiments are as follows:

[0038] (1) The octafluorocyclopentene raw material enters the vaporizer E1101, and the operating pressure of E1101 is 0.12 - 0.3 MPa and the temperature is 30 - 60 °C; the vaporized material enters the adsorption column X1101.

[0039] (2) The operating pressure of the adsorption column X1101 is 0.12 - 0.3 MPa and the temperature is 30 - 60 °C, and the material after the action of the adsorption column enters the extractive distillation column T1201.

[0040] The adsorbent filled in the adsorption column X1101 is one or a mixture of molecular sieve adsorbent 13X, molecular sieve adsorbent HZSM-5, and high-silica zeolite.

[0041] (3) The operating pressure of the extractive distillation column is 0.12 - 0.2 MPa and the temperature is 30 - 160 °C. The crude octafluorocyclopentene is taken out from the top of the extractive distillation column, and the extractant fraction is taken out from the bottom of the column;

[0042] The extractant used in the extractive distillation column T1201 is one or a mixture of acetonitrile, DMF, and methyl isobutyl ketone.

[0043] The mass ratio of the extractant to the octafluorocyclopentene material in the extractive distillation column T1201 is 5 - 15:1.

[0044] (4) Feed the crude octafluorocyclopentene obtained in step (3) to the light component removal column T1301, with an operating pressure of 0.12 - 0.2 MPa and a temperature of 30 - 160 °C. Light components are taken from the top of the column, and the octafluorocyclopentene fraction is taken from the bottom of the column.

[0045] (5) Feed the octafluorocyclopentene fraction prepared in step (4) to the heavy component removal column T1401, with an operating pressure of 0.12 - 0.2 MPa and a temperature of 30 - 160 °C. The electronic grade octafluorocyclopentene product is taken from the top of the column, and the heavy components are taken from the bottom of the column.

[0046] (6) Feed the extractant fraction prepared in step (3) to the extractant recovery column T1501, with an operating pressure of 0.12 - 0.2 MPa and a temperature of 30 - 160 °C. Light components are taken from the top of the column, and the extractant is taken from the bottom of the column.

[0047] The purity of the electronic grade octafluorocyclopentene product prepared by the present invention is ≥ 5N, and the yield is ≥ 95%.

[0048] A refining device for electronic grade octafluorocyclopentene, comprising a vaporizer E1101, an adsorption tower X1101, an extractive distillation column T1201, a light component removal column T1301, a heavy component removal column T1401, and an extractant recovery column T1501 that are connected in sequence according to the reaction order;

[0049] The top of the vaporizer E1101 is connected to the adsorption tower X1101;

[0050] The top of the extractive distillation column T1201 is connected to the light component removal column T1301, and the bottom of the light component removal column T1301 is connected to the heavy component removal column T1401;

[0051] The extractant recovery column T1501 is connected to the bottom of the extractive distillation column T1201.

[0052] The following further illustrates the present invention in conjunction with the attached Figure 1 drawings and specific embodiments.

[0053] Example 1

[0054] Octafluorocyclopentene raw material is transported to vaporizer E1101 at a feeding rate of 1 kg / h, vaporized under the conditions of a pressure of 0.3 MPa and a temperature of 47 °C, and then transported to adsorption tower X1101. The adsorption tower X1101 is filled with 13X molecular sieve, with an operating pressure of 0.25 MPa and an operating temperature of 50 °C. After the CH impurities in the raw material are removed by the action of the adsorption tower X1101, it enters the extractive distillation tower T1201. The extractant used in the extractive distillation tower T1201 is acetonitrile, and the mass ratio of the extractant to the octafluorocyclopentene raw material after adsorption is 5:1. The feeding rate of the extractant to the extractive distillation tower is 5 kg / h, with an operating pressure of 0.2 MPa and an operating temperature of 40 - 110 °C. The crude distillate of octafluorocyclopentene is taken out from the top of the tower and enters the light component removal tower T1301, and the extractant distillate is taken out from the bottom of the tower and enters the extractant recovery tower T1501. The light component removal tower T1301 has an operating pressure of 0.2 MPa and an operating temperature of 40 - 110 °C. Light impurities such as hydrogen, oxygen, and nitrogen are taken out from the top of the tower, and the material taken out from the bottom of the tower enters the heavy component removal tower T1401. The heavy component removal tower T1401 has an operating pressure of 0.2 MPa and an operating temperature of 40 - 110 °C. The 5N octafluorocyclopentene product is taken out from the top of the tower, and acetonitrile is taken out from the bottom of the tower. The extractant recovery tower T1501 has an operating pressure of 0.2 MPa and an operating temperature of 40 - 110 °C. Impurities such as octafluorocyclopentene and perfluorocyclopentane are taken out from the top of the tower, and acetonitrile taken out from the bottom of the tower is returned to the extractive distillation tower T1201.

[0055] The purity of the electronic-grade octafluorocyclopentene product prepared in this example is ≥5N, and the yield is 97.3%.

[0056] Example 2

[0057] Octafluorocyclopentene raw material is transported to vaporizer E1101 at a feeding rate of 1 kg / h, vaporized under the conditions of a pressure of 0.2 MPa and a temperature of 39 °C, and then transported to adsorption tower X1101. The adsorption tower X1101 is filled with HZSM-5 molecular sieve, with an operating pressure of 0.15 MPa and an operating temperature of 60 °C. After removing CH impurities in the raw material through the action of the adsorption tower X1101, it enters the extractive distillation tower T1201. The extractant used in the extractive distillation tower T1201 is DMF. The mass ratio of the extractant to the octafluorocyclopentene raw material after adsorption is 10:1. The feeding rate of the extractant to the extractive distillation tower is 10 kg / h, with an operating pressure of 0.12 MPa and an operating temperature of 30 - 160 °C. The crude distillate of octafluorocyclopentene is taken from the top of the tower and enters the light component removal tower T1301, and the extractant distillate is taken from the bottom of the tower and enters the extractant recovery tower T1501. The light component removal tower T1301 has an operating pressure of 0.12 MPa and an operating temperature of 30 - 160 °C. Light impurities such as hydrogen, oxygen, and nitrogen are taken from the top of the tower, and the material taken from the bottom of the tower enters the heavy component removal tower T1401. The heavy component removal tower T1401 has an operating pressure of 0.12 MPa and an operating temperature of 30 - 160 °C. The 5N octafluorocyclopentene product is taken from the top of the tower, and DMF is taken from the bottom of the tower. The extractant recovery tower T1501 has an operating pressure of 0.12 MPa and an operating temperature of 30 - 160 °C. Impurities such as octafluorocyclopentene and perfluorocyclopentane are taken from the top of the tower, and DMF taken from the bottom of the tower is returned to the extractive distillation tower T1201.

[0058] The purity of the electronic-grade octafluorocyclopentene product prepared in this example is ≥5N, and the yield is 97.0%.

[0059] Example 3

[0060] Octafluorocyclopentene raw material is fed to vaporizer E1101 at a feeding rate of 1 kg / h, vaporized under the conditions of a pressure of 0.12 MPa and a temperature of 30 °C, and then fed to adsorption tower X1101. Adsorption tower X1101 is filled with high-silica zeolite, with an operating pressure of 0.12 MPa and an operating temperature of 30 °C. After the CH impurities in the raw material are removed by the action of adsorption tower X1101, it enters extraction and rectification tower T1201. The extraction agent used in extraction and rectification tower T1201 is methyl isobutyl ketone. The mass ratio of the extraction agent to the octafluorocyclopentene raw material after adsorption is 15:1. The feeding rate of the extraction agent to extraction and rectification tower is 15 kg / h, with an operating pressure of 0.12 MPa and an operating temperature of 30 - 118 °C. The crude fraction of octafluorocyclopentene is taken out from the top of the tower and enters light component removal tower T1301, and the extraction agent fraction is taken out from the bottom of the tower and enters extraction agent recovery tower T1501. Light component removal tower T1301 has an operating pressure of 0.12 MPa and an operating temperature of 30 - 118 °C. Light impurities such as hydrogen, oxygen, and nitrogen are taken out from the top of the tower, and the material taken out from the bottom of the tower enters heavy component removal tower T1401. Heavy component removal tower T1401 has an operating pressure of 0.12 MPa and an operating temperature of 30 - 118 °C. 5N octafluorocyclopentene product is taken out from the top of the tower, and methyl isobutyl ketone is taken out from the bottom of the tower. Extraction agent recovery tower T1501 has an operating pressure of 0.12 MPa and an operating temperature of 40 - 118 °C. Impurities such as octafluorocyclopentene and perfluorocyclopentane are taken out from the top of the tower, and methyl isobutyl ketone taken out from the bottom of the tower is returned to extraction and rectification tower T1201.

[0061] The purity of the electronic-grade octafluorocyclopentene product prepared in this example is ≥5N, and the yield is 97.1%.

[0062] Example 4

[0063] Octafluorocyclopentene raw material is fed to vaporizer E1101 at a feeding rate of 1 kg / h, vaporized under the conditions of a pressure of 0.15 MPa and a temperature of 60 °C, and then fed to adsorption tower X1101. Adsorption tower X1101 is filled with high-silica zeolite, with an operating pressure of 0.3 MPa and an operating temperature of 40 °C. After the CH impurities in the raw material are removed by the action of adsorption tower X1101, it enters extractive distillation tower T1201. The extractant used in extractive distillation tower T1201 is methyl isobutyl ketone, and the mass ratio of the extractant to the octafluorocyclopentene raw material after adsorption is 8:1. The feeding rate of the extractant to the extractive distillation tower is 15 kg / h, with an operating pressure of 0.15 MPa and an operating temperature of 30 - 118 °C. The crude distillate of octafluorocyclopentene is taken out from the top of the tower and enters de-light tower T1301, and the extractant distillate is taken out from the bottom of the tower and enters extractant recovery tower T1501. De-light tower T1301 has an operating pressure of 0.15 MPa and an operating temperature of 30 - 118 °C. Light impurities such as hydrogen, oxygen, and nitrogen are taken out from the top of the tower, and the material taken out from the bottom of the tower enters de-heavy tower T1401. De-heavy tower T1401 has an operating pressure of 0.15 MPa and an operating temperature of 30 - 118 °C. The 5N octafluorocyclopentene product is taken out from the top of the tower, and methyl isobutyl ketone is taken out from the bottom of the tower. Extractant recovery tower T1501 has an operating pressure of 0.15 MPa and an operating temperature of 40 - 118 °C. Impurities such as octafluorocyclopentene and perfluorocyclopentane are taken out from the top of the tower, and methyl isobutyl ketone taken out from the bottom of the tower is returned to extractive distillation tower T1201.

[0064] The purity of the electronic-grade octafluorocyclopentene product prepared in this example is ≥5N, and the yield is 97.6%.

[0065] Example 5

[0066] Octafluorocyclopentene raw material is transported to vaporizer E1101 at a feeding rate of 1 kg / h, vaporized under the conditions of a pressure of 0.12 MPa and a temperature of 30 °C, and then transported to adsorption tower X1101. Adsorption tower X1101 is filled with HZSM-5 molecular sieve, 13X molecular sieve and high-silica zeolite, and the volume ratio of the three is 1:1:1. The operating pressure is 0.12 MPa and the operating temperature is 30 °C. After the raw material is purified by adsorption tower X1101 to remove CH impurities, it enters extractive distillation tower T1201. The extractants used in extractive distillation tower T1201 are methyl isobutyl ketone and DMF, and the mass ratio of the two is 1:1. The mass ratio of the sum of the masses of the two extractants to the mass of the octafluorocyclopentene raw material after adsorption is 15:1. The feeding rate of the extractant in extractive distillation tower T1201 is 15 kg / h, the operating pressure is 0.12 MPa, and the operating temperature is 30 - 118 °C. The crude fraction of octafluorocyclopentene is taken from the top of the tower and enters de-light tower T1301, and the extractant fraction is taken from the bottom of the tower and enters extractant recovery tower T1501. The operating pressure of de-light tower T1301 is 0.12 MPa, and the operating temperature is 30 - 118 °C. Light impurities such as hydrogen, oxygen, and nitrogen are taken from the top of the tower, and the material at the bottom of the tower enters de-heavy tower T1401. The operating pressure of de-heavy tower T1401 is 0.12 MPa, and the operating temperature is 30 - 118 °C. 5N octafluorocyclopentene product is taken from the top of the tower, and methyl isobutyl ketone is taken from the bottom of the tower. The operating pressure of extractant recovery tower T1501 is 0.12 MPa, and the operating temperature is 40 - 118 °C. Impurities such as octafluorocyclopentene and perfluorocyclopentane are taken from the top of the tower, and methyl isobutyl ketone taken from the bottom of the tower is returned to extractive distillation tower T1201.

[0067] The purity of the electronic-grade octafluorocyclopentene product prepared in this example is ≥5N, and the yield is 98.8%.

[0068] For the technical solutions disclosed and proposed in the present invention, those skilled in the art can achieve them by referring to the content of this article and appropriately changing conditions, routes and other links. Although the methods and preparation technologies of the present invention have been described through preferred embodiments, it is obvious that relevant technical personnel can make changes or re-combinations to the methods and technical routes described in this article without departing from the content, spirit and scope of the present invention to achieve the final preparation technology. It should be particularly noted that all similar substitutions and modifications are obvious to those skilled in the art, and they are all regarded as being included in the spirit, scope and content of the present invention.

Claims

1. A refining method for electronic-grade octafluorocyclopentene, characterized in that, It includes the following steps: (1) Vaporize the octafluorocyclopentene raw material; (2) Adsorb the vaporized octafluorocyclopentene raw material with an adsorbent; (3) After adsorption, the adsorbed octafluorocyclopentene raw material is obtained. Add an extractant to the adsorbed octafluorocyclopentene raw material for extractive distillation. The crude octafluorocyclopentene fraction is taken from the top of the extractive distillation process, and the extractant fraction is taken from the bottom of the column; (4) Subject the crude octafluorocyclopentene fraction obtained in step (3) to light component removal distillation. The light components are taken from the top of the column, and the octafluorocyclopentene fraction is taken from the bottom of the column; (5) Subject the octafluorocyclopentene fraction prepared in step (4) to heavy component removal distillation. The electronic grade octafluorocyclopentene product is taken from the top of the column, and the heavy components are taken from the bottom of the column.

2. The refining method of electronic-grade octafluorocyclopentene according to claim 1, characterized in that, It also includes the following steps: (6) Feed the extractant fraction prepared in step (3) for extractant rectification recovery. The light components are taken from the top of the column, and the extractant is taken from the bottom of the column.

3. The refining method of electronic-grade octafluorocyclopentene according to claim 1, characterized in that, The vaporization operation pressure in step (1) is 0.12 - 0.3 MPa, and the temperature is 30 - 60 °C; The adsorption operation pressure in step (2) is 0.12 - 0.3 MPa, and the temperature is 30 - 60 °C; The extractive distillation operation pressure in step (3) is 0.12 - 0.2 MPa, and the temperature is 30 - 160 °C; The light component removal distillation operation pressure in step (4) is 0.12 - 0.2 MPa, and the temperature is 30 - 160 °C; The heavy component removal distillation operation pressure in step (5) is 0.12 - 0.2 MPa, and the temperature is 30 - 160 °C.

4. The refining method of electronic-grade octafluorocyclopentene according to claim 2, characterized in that, The extractant rectification recovery operation pressure in step (6) is 0.12 - 0.2 MPa, and the temperature is 30 - 160 °C.

5. The refining method of electronic-grade octafluorocyclopentene according to claim 1, characterized in that, The adsorbent used in step (2) is one or a mixture of molecular sieve adsorbents 13X, molecular sieve adsorbent HZSM-5, and high-silica zeolite.

6. The refining method of electronic-grade octafluorocyclopentene according to claim 1, characterized in that, The extractant used in the extractive distillation in step (3) is one or a mixture of acetonitrile, DMF, and methyl isobutyl ketone.

7. The refining method of electronic-grade octafluorocyclopentene according to claim 1, characterized in that, The mass ratio of the extractant to the adsorbed octafluorocyclopentene raw material in step (3) is 5 - 15:

1.

8. The refining method of electronic-grade octafluorocyclopentene according to claim 1, characterized in that, The purity of the produced electronic grade octafluorocyclopentene product is ≥5N, and the yield is ≥95%.

9. A refining device for electronic-grade octafluorocyclopentene, which is used for the refining method of electronic-grade octafluorocyclopentene according to any one of claims 1-8, and is characterized in that, It includes a vaporizer (E1101), an adsorption tower (X1101), an extractive distillation tower (T1201), a light component removal tower (T1301), and a heavy component removal tower (T1401) connected in sequence according to the reaction order; The top of the vaporizer (E1101) is connected to the adsorption tower (X1101); The top of the extractive distillation tower (T1201) is connected to the light component removal tower (T1301), and the bottom of the light component removal tower (T1301) is connected to the heavy component removal tower (T1401).

10. The refining device for electronic-grade octafluorocyclopentene according to claim 9, characterized in that, It also includes an extractant recovery tower (T1501), and the extractant recovery tower (T1501) is connected to the bottom of the extractive distillation tower (T1201).

Citation Information

Patent Citations

  • Preparation method of octafluorocyclopentene

    CN107188778A

  • An industrial production method for octafluorocyclopentene

    CN108276243B

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