CN114478613A - Method for simultaneously removing high-boiling-point substances and low-boiling-point substances in organic silicon crude monomer - Google Patents
Method for simultaneously removing high-boiling-point substances and low-boiling-point substances in organic silicon crude monomer Download PDFInfo
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- CN114478613A CN114478613A CN202210138155.6A CN202210138155A CN114478613A CN 114478613 A CN114478613 A CN 114478613A CN 202210138155 A CN202210138155 A CN 202210138155A CN 114478613 A CN114478613 A CN 114478613A
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- 239000000126 substance Substances 0.000 title claims abstract description 50
- 239000000178 monomer Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title description 5
- 229910052710 silicon Inorganic materials 0.000 title description 5
- 239000010703 silicon Substances 0.000 title description 5
- 238000005192 partition Methods 0.000 claims abstract description 37
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000009835 boiling Methods 0.000 claims description 22
- 238000007599 discharging Methods 0.000 claims description 10
- 238000004891 communication Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 12
- 239000005051 trimethylchlorosilane Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 2
- 239000005046 Chlorosilane Substances 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- VNJCDDZVNHPVNM-UHFFFAOYSA-N chloro(ethyl)silane Chemical compound CC[SiH2]Cl VNJCDDZVNHPVNM-UHFFFAOYSA-N 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- FBBDOOHMGLLEGJ-UHFFFAOYSA-N methane;hydrochloride Chemical compound C.Cl FBBDOOHMGLLEGJ-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses a method for simultaneously removing high-boiling-point substances and low-boiling-point substances in an organosilicon crude monomer, which comprises the following steps: introducing an organosilicon crude monomer into one side of a partition plate of a partition wall tower, separating low-boiling-point substances and monomethyl trichlorosilane at the upper part of the partition wall tower, separating high-boiling-point substances and dimethyl dichlorosilane at the lower part of the partition wall tower, and extracting monomethyl trichlorosilane and dimethyl dichlorosilane at the other side of the partition plate. On the premise of achieving the same separation purity, the method of the invention saves energy consumption by more than 15% compared with the traditional rectification, can reduce the investment and the occupied area of three devices, reduces the equipment investment by more than 5%, and can simplify the process.
Description
Technical Field
The invention belongs to the technical field of organosilicon purification, and particularly relates to a method for simultaneously removing high-boiling-point substances and low-boiling-point substances in organosilicon crude monomers.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
In addition to monomethyltrichlorosilane, dimethyldichlorosilane, trimethylchlorosilane, monomethylhydrochlorosilane and other monomers, low-boiling-point substances such as tetramethylsilane and hydrochlorosilane, and high-boiling-point substances such as ethylchlorosilane and alkyldisilane are also contained in reaction products in the production process of organic silicon. The traditional separation process is to remove high-boiling-point substances and then remove low-boiling-point substances, and then to separate each monomer one by one. The height removing tower and the lower removing tower of the traditional rectification process are both about 70 meters, and the energy consumption is very high.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for simultaneously removing high-boiling-point substances and low-boiling-point substances in organosilicon crude monomers.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for simultaneously removing high-boiling-point substances and low-boiling-point substances in organosilicon crude monomers comprises the following steps:
introducing an organosilicon crude monomer into one side of a partition plate of a partition wall tower, separating low-boiling-point substances and monomethyl trichlorosilane at the upper part of the partition wall tower, separating high-boiling-point substances and dimethyl dichlorosilane at the lower part of the partition wall tower, and extracting monomethyl trichlorosilane and dimethyl dichlorosilane at the other side of the partition plate.
The above one or more embodiments of the present invention achieve the following advantageous effects:
the dividing wall tower can fully separate low-boiling-point substances such as trimethylchlorosilane, the content of the low-boiling-point substances such as the trimethylchlorosilane in the monomethyltrichlorosilane and the dimethyldichlorosilane extracted from the right side of the middle part of the dividing wall tower is below 0.03 percent, and after the monomethyltrichlorosilane and the dimethyldichlorosilane are further separated in the binary A tower, the monomethyltrichlorosilane with the content of more than 99.5 percent can be obtained from the tower top, wherein the content of the trimethylchlorosilane is below 0.2 percent. The dividing wall tower can also realize the separation of dimethyldichlorosilane and heavy components, the content of high-boiling-point substances in the monomethyltrichlorosilane and dimethyldichlorosilane extracted from the right side of the middle part of the dividing wall tower is below 0.034%, and after the binary tower is further separated, the dimethyldichlorosilane with the content of more than 99.95% can be obtained at the bottom of the tower, wherein the content of the heavy components is below 0.035%.
The invention can obviously reduce the energy consumption and equipment investment of the rectification of the organic silicon monomer, saves the energy consumption by more than 15 percent compared with the traditional rectification on the premise of achieving the same separation purity, can reduce the investment and the occupied area of three pieces of equipment, can reduce the equipment investment by more than 5 percent, and can simplify the flow.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic illustration of a dividing wall column feed configuration according to one or more embodiments of the present invention.
In the figure: the mutual spacing or size is exaggerated to show the position of each part, and the schematic diagram is only used for illustration;
wherein, the flow: 1. organosilicon crude monomer feed, 2, light components, 3, a mixture of dimethyldichlorosilane and monomethyltrichlorosilane, 4, heavy components.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
A method for simultaneously removing high-boiling-point substances and low-boiling-point substances in organosilicon crude monomers comprises the following steps:
introducing an organosilicon crude monomer into one side of a partition plate of a partition wall tower, separating low-boiling-point substances and monomethyl trichlorosilane at the upper part of the partition wall tower, separating high-boiling-point substances and dimethyl dichlorosilane at the lower part of the partition wall tower, and extracting monomethyl trichlorosilane and dimethyl dichlorosilane at the other side of the partition plate.
In some embodiments, the interior of the divided wall column is divided into four regions, an upper communication region, a lower communication region, a feed region, and a discharge region, the upper communication region being located above the dividing wall, the lower communication region being located below the dividing wall, the feed region and the discharge region being located on either side of the dividing wall.
Furthermore, according to the content of each component in the feeding material and the separation difficulty, the ratio of the distance between the partition plate and the tower wall on the feeding side to the distance between the partition plate and the tower wall on the discharging side is 0.4-0.7: 1.
Further, the feed inlet is positioned at 20-65% of the height of the feeding area.
Furthermore, the discharge ports are positioned at 60-85% of the height of the discharge area, and the discharge ports are arranged in the ascending order from top to bottom so as to control the content of heavy components in the discharge.
Further, the ratio of the liquid flow rates from the upper communicating zone into the feeding zone and the discharging zone is 0.1-0.4: 1.
In some embodiments, the temperature of the crude silicone monomer entering the divided wall column is from 10 to 80 ℃.
In some embodiments, the composition of the feed to the dividing wall column is in the range of 4-15% for the light components, 70-95% for the monomethyltrichlorosilane and dimethyldichlorosilane, and 1-15% for the heavy components.
In some embodiments, the theoretical number of stages of the divided wall column is 50-75% of the theoretical number of stages of the connected column.
In some embodiments, the reflux ratio of the divided wall column ranges from 70 to 110.
In some embodiments, the liquid flow ratio into the feed zone and the discharge zone from the upper communicating zone is from 0.1 to 0.4:1 and the gas flow ratio into the feed zone and the discharge zone from the lower communicating zone is from 0.4 to 0.75: 1.
The present invention will be further described with reference to the following specific examples.
The partition tower is utilized to simultaneously remove high-boiling residues and low-boiling residues in the organic silicon monomer, trimethylchlorosilane and other light components can be directly removed from the top of the partition tower, high-boiling residues heavier than dimethyldichlorosilane can be removed from the tower kettle, and monomethyltrichlorosilane and dimethyldichlorosilane can be directly extracted from the middle part of the partition tower.
The dividing wall tower is divided into four parts: the upper communicating area, the lower communicating area and the middle part are divided into a left part and a right part by a clapboard. The ratio of the distance between the partition board and the tower wall at the feeding side to the distance between the partition board and the tower wall at the discharging side is 0.4-0.7: 1; the feed inlet is positioned at the position of 20-65% of the height of the feed area; the discharge hole is positioned at 60-85% of the height of the discharge area; the liquid flow ratio entering the feeding zone and the discharging zone from the upper communicating zone is 0.1-0.4: 1.
The feed composition is shown in table 1, with a capacity of 10 ten thousand tons per year. The area ratio of the left and right sides of the partition was 0.46, the feed position was 55% of the height of the left side, and the take-off positions of dimethyldichlorosilane and monomethyltrichlorosilane were 79% of the height of the right side.
The feeding temperature is 25 ℃, the extraction ratio at the top of the tower is 5.67 percent, and the reflux ratio is 90; the side mining proportion is 91.33%. The ratio of the liquid flow rate from the communicating column to the feed side and the take-off side was 0.247, and the ratio of the gas flow rate from the communicating column to the feed side and the take-off side was 0.57.
TABLE 1 organosilicon crude monomer feed composition
| Components | Mass percent of |
| Methane chloride | 0.003 |
| |
0.004 |
| Tetramethylsilane | 0.27 |
| Trichlorosilane | 0.02 |
| Dimethyl hydrogen chlorosilane | 0.37 |
| Methyl hydrochlorosilane | 1.2 |
| |
0.02 |
| Tetrachlorosilane | 0.08 |
| Trimethylchlorosilane | 5.9 |
| |
0.002 |
| Monomethyl trichlorosilane | 6.46 |
| Dimethyldichlorosilane | 85.37 |
| High boiling substance | 2.682 |
| Total of | 100.000 |
Table 2 shows the purity of the separation achieved in this example and in conventional rectification. Table 3 shows the same capacity, the example and the equipment specifications for conventional rectification when this purity is achieved.
TABLE 2 product purity of this example and conventional rectification
TABLE 3 Equipment Specifications for this example and for conventional rectification
| Partition tower | High tower takes off | Delow tower | |
| Tower warp, m | 3.4 | 3.2 | 2.2 |
| Tangent height, m | 98 | 66 | 68 |
When the product purity listed in Table 2 is reached, the embodiment can save 17.4% of steam and 17.7% of circulating water compared with the traditional rectification. The steam price is calculated according to 220 yuan/ton, and 880 ten thousand yuan of operating cost can be saved each year.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for simultaneously removing high-boiling-point substances and low-boiling-point substances in an organosilicon crude monomer is characterized by comprising the following steps: the method comprises the following steps:
introducing an organosilicon crude monomer into one side of a partition plate of a partition wall tower, separating low-boiling-point substances and monomethyl trichlorosilane at the upper part of the partition wall tower, separating high-boiling-point substances and dimethyl dichlorosilane at the lower part of the partition wall tower, and extracting monomethyl trichlorosilane and dimethyl dichlorosilane at the other side of the partition plate.
2. The method for simultaneously removing high-boiling substances and low-boiling substances in crude organosilicon monomer according to claim 1, wherein the method comprises the following steps: the inside of the partition tower is divided into four areas, namely an upper communication area, a lower communication area, a feeding area and a discharging area, wherein the upper communication area is positioned above the partition plate, the lower communication area is positioned below the partition plate, and the feeding area and the discharging area are respectively positioned at two sides of the partition plate.
3. The method for simultaneously removing high-boiling substances and low-boiling substances in crude organosilicon monomers as claimed in claim 2, wherein: the ratio of the distance between the partition board and the tower wall at the feeding side to the distance between the partition board and the tower wall at the discharging side is 0.4-0.7: 1.
4. The method for simultaneously removing high-boiling substances and low-boiling substances in crude organosilicon monomers as claimed in claim 2, wherein: the feed inlet is positioned at 20-65% of the height of the feeding area.
5. The method for simultaneously removing high-boiling substances and low-boiling substances in crude organosilicon monomers as claimed in claim 2, wherein: the discharge hole is positioned at 60-85% of the height of the discharge area.
6. The method for simultaneously removing high-boiling substances and low-boiling substances in crude organosilicon monomers as claimed in claim 2, wherein: the liquid flow ratio entering the feeding zone and the discharging zone from the upper communicating zone is 0.1-0.4: 1.
7. The method for simultaneously removing high-boiling substances and low-boiling substances in crude organosilicon monomers as claimed in claim 1, wherein: the temperature of the organosilicon crude monomer entering the dividing wall tower is 10-80 ℃.
8. The method for simultaneously removing high-boiling substances and low-boiling substances in crude organosilicon monomers as claimed in claim 1, wherein: in the feed composition of the partition wall tower, the composition range of light components is 4-15%, the composition range of monomethyl trichlorosilane and dimethyl dichlorosilane is 70-95%, and the composition range of heavy components is 1-15%.
9. The method for simultaneously removing high-boiling substances and low-boiling substances in crude organosilicon monomers as claimed in claim 1, wherein: the theoretical stage number of the partition wall tower is 50-75% of that of the communicating tower;
preferably, the reflux ratio of the divided wall column is in the range of 70 to 110.
10. The method for simultaneously removing high-boiling substances and low-boiling substances in crude organosilicon monomers as claimed in claim 1, wherein: the liquid flow ratio entering the feeding zone and the discharging zone from the upper communicating zone is 0.1-0.4:1, and the gas flow ratio entering the feeding zone and the discharging zone from the lower communicating zone is 0.4-0.75: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210138155.6A CN114478613B (en) | 2022-02-15 | Method for simultaneously removing high-boiling-point substances and low-boiling-point substances in crude organosilicon monomers |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210138155.6A CN114478613B (en) | 2022-02-15 | Method for simultaneously removing high-boiling-point substances and low-boiling-point substances in crude organosilicon monomers |
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| Publication Number | Publication Date |
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| CN114478613A true CN114478613A (en) | 2022-05-13 |
| CN114478613B CN114478613B (en) | 2024-10-25 |
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Cited By (2)
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| CN115043869A (en) * | 2022-06-08 | 2022-09-13 | 宁夏福瑞硅烷材料有限公司 | Method for preparing high-purity vinyl trimethoxy silane |
| CN115317944A (en) * | 2022-07-29 | 2022-11-11 | 华陆工程科技有限责任公司 | Separation method of organic silicon ring body mixture |
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| CN115043869A (en) * | 2022-06-08 | 2022-09-13 | 宁夏福瑞硅烷材料有限公司 | Method for preparing high-purity vinyl trimethoxy silane |
| CN115317944A (en) * | 2022-07-29 | 2022-11-11 | 华陆工程科技有限责任公司 | Separation method of organic silicon ring body mixture |
| CN115317944B (en) * | 2022-07-29 | 2023-10-20 | 华陆工程科技有限责任公司 | Separation method of organosilicon ring body mixture |
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