CN111875481A - Continuous production process and equipment for dihydric alcohol vinyl ether - Google Patents
Continuous production process and equipment for dihydric alcohol vinyl ether Download PDFInfo
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- CN111875481A CN111875481A CN202010849346.4A CN202010849346A CN111875481A CN 111875481 A CN111875481 A CN 111875481A CN 202010849346 A CN202010849346 A CN 202010849346A CN 111875481 A CN111875481 A CN 111875481A
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 108
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000010924 continuous production Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 113
- 239000003054 catalyst Substances 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 34
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 167
- 238000000926 separation method Methods 0.000 claims description 83
- 239000007788 liquid Substances 0.000 claims description 64
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 44
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 42
- 239000012295 chemical reaction liquid Substances 0.000 claims description 14
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 13
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 13
- HMBNQNDUEFFFNZ-UHFFFAOYSA-N 4-ethenoxybutan-1-ol Chemical compound OCCCCOC=C HMBNQNDUEFFFNZ-UHFFFAOYSA-N 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 6
- 150000002009 diols Chemical class 0.000 claims description 3
- 230000004913 activation Effects 0.000 abstract description 2
- 230000018044 dehydration Effects 0.000 abstract description 2
- 238000006297 dehydration reaction Methods 0.000 abstract description 2
- 238000007086 side reaction Methods 0.000 abstract description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 abstract 1
- 239000005977 Ethylene Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- -1 surface protection Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/05—Preparation of ethers by addition of compounds to unsaturated compounds
- C07C41/06—Preparation of ethers by addition of compounds to unsaturated compounds by addition of organic compounds only
- C07C41/08—Preparation of ethers by addition of compounds to unsaturated compounds by addition of organic compounds only to carbon-to-carbon triple bonds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a continuous production process and equipment of dihydric alcohol vinyl ether, belonging to the technical field of chemical material preparation. The invention adds the dihydric alcohol and the ethylene into the continuous production equipment, thereby realizing the continuous production of the dihydric alcohol vinyl ether. The invention not only realizes the continuous production of the dihydric alcohol vinyl ether, but also greatly improves the production efficiency, ensures that the reaction which takes longer time can be completed in a short time, and simultaneously ensures the stability of the product. Moreover, the catalyst dehydration activation method provided by the invention obviously improves the reaction rate, greatly reduces the occurrence of side reactions and improves the yield.
Description
Technical Field
The invention belongs to the technical field of petrochemical industry, and particularly relates to a continuous production process of dihydric alcohol vinyl ether.
Background
The dihydric alcohol vinyl ether is used as an important chemical raw material, has ether bond and double bond in the molecular structure, has very unique service performance, is an important organic synthetic intermediate and functional polymeric monomer, and the homopolymer and the copolymer thereof are widely applied to a plurality of fields such as adhesive, coating, lubricant, plasticizer, insecticide, surface protection, material and the like. The research in the aspect of synthesizing the dihydric alcohol vinyl ether in China is started late, no mature industrial production exists so far, relevant research reports are rarely seen, and most of the commercial products are imported and subpackaged abroad. At present, only German BASF company, American ISP company and Japan Bolus petrochemical company produce the product, and most of the preparation methods are applied for patent protection.
At present, the traditional production process of the dihydric alcohol still adopts the traditional intermittent production process which is intermittent feeding and discharging, and has low production efficiency, inconvenient operation and unstable product quality. One of the raw materials, acetylene, is fed in a bubbling mode, is operated under normal pressure or slight negative pressure, takes longer reaction time, needs more than 12 hours to reach reaction equilibrium, thereby resulting in very low generation efficiency and larger amount of by-products due to longer reaction time. In order to improve the yield, a multi-kettle parallel connection mode can be adopted, so that the equipment investment is increased, and a larger generation operation space is occupied.
Disclosure of Invention
The invention aims to provide a continuous production process of dihydric alcohol.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a continuous production process of dihydric alcohol vinyl ether, which comprises the following steps:
(1) adding potassium hydroxide and dihydric alcohol into a catalyst preparation kettle (1), heating to 50-180 ℃, reducing the pressure to-0.05-0.1 mpa, and reacting for 0.1-2 h to obtain a catalyst;
(2) injecting the catalyst into an alcohol ether reaction kettle (2), introducing acetylene gas into the alcohol ether reaction kettle (2) under the condition of stirring, controlling the pressure to be 0-5mpa, and slowly heating to 80-180 ℃ to obtain a reaction solution;
(3) the reaction liquid is conveyed to a gas-liquid separation tank (3), the separated gas is conveyed back to the alcohol ether reaction kettle (2), and the separated liquid is conveyed to a separation tower (4);
(4) the tower bottom material in the separation tower (4) is conveyed back to the alcohol ether reaction kettle (2), fresh dihydric alcohol is supplemented according to the liquid level of the alcohol ether reaction kettle (2) to stabilize the liquid level at 70-80%, and the tower top material in the separation tower (4) is conveyed to the light component removal tower (5);
(5) and (3) treating the material at the top of the tower by a light component removal tower (5), and conveying the material to a heavy component removal tower (6) to obtain the dihydric alcohol vinyl ether.
Preferably, the diol is one of ethylene glycol, diethylene glycol and 1, 4-butanediol.
Preferably, the ratio of the glycol: the ratio of potassium hydroxide is 100: 1-50.
Preferably, the alcohol ether reaction kettle is a self-suction reaction kettle.
Preferably, the self-priming reaction kettle controls the liquid level and the pressure to be constant through the feeding of fresh alcohol and acetylene gas.
Preferably, the treatment device of the production process comprises a catalyst preparation kettle (1), and a discharge hole of the catalyst reaction kettle (1) is communicated with a feed hole of the alcohol ether reaction kettle (2);
the discharge hole of the alcohol ether reaction kettle (2) is communicated with the feed inlet of the gas-liquid separation tank (3), and the gas outlet of the gas-liquid separation tank (3) is communicated with the gas inlet of the alcohol ether reaction kettle (2);
a discharge hole of the gas-liquid separation tank (3) is communicated with a feed inlet of the separation tower (4), and a discharge hole at the bottom of the separation tower (4) is communicated with a feed inlet of the alcohol ether reaction kettle (2);
the discharge port of the top of the separation tower (4) is communicated with the feed port of the light component removal tower (5), and the discharge port of the light component removal tower (5) is communicated with the feed port of the heavy component removal tower (6).
In addition, the invention provides a continuous production process of 1, 4-butanediol vinyl ether, which comprises the following steps:
(1) adding potassium hydroxide and 1, 4-butanediol into a catalyst preparation kettle (1), heating to 130 ℃, reducing the pressure to-0.08 mpampa, and reacting for 0.5h to obtain a catalyst; according to the mass ratio, the ratio of 1, 4-butanediol: potassium hydroxide is 100: 8;
(2) injecting the catalyst into an alcohol ether reaction kettle (2), introducing acetylene gas into the alcohol ether reaction kettle (2) under the condition of stirring, boosting the pressure to 0.35mpa, and slowly heating to 140 ℃ to obtain a reaction solution; the alcohol ether reaction kettle is a self-suction reaction kettle;
(3) the reaction liquid is conveyed to a gas-liquid separation tank (3), the separated gas is conveyed back to the alcohol ether reaction kettle (2), and the separated liquid is conveyed to a separation tower (4);
(4) the tower bottom material in the separation tower (4) is conveyed back to the alcohol ether reaction kettle (2), fresh 1, 4-butanediol is supplemented according to the liquid level of the alcohol ether reaction kettle (2) to stabilize the liquid level at 70% -80%, and the tower top material in the separation tower (4) is conveyed to the light component removal tower (5);
(5) the material at the top of the tower is treated by a light component removing tower (5) and then is conveyed to a heavy component removing tower (6) to obtain 1,4 butanediol vinyl ether;
the treatment device of the production process comprises a catalyst preparation kettle (1), wherein a discharge hole of the catalyst reaction kettle (1) is communicated with a feed hole of the alcohol ether reaction kettle (2);
the discharge hole of the alcohol ether reaction kettle (2) is communicated with the feed inlet of the gas-liquid separation tank (3), and the gas outlet of the gas-liquid separation tank (3) is communicated with the gas inlet of the alcohol ether reaction kettle (2);
a discharge hole of the gas-liquid separation tank (3) is communicated with a feed inlet of the separation tower (4), and a discharge hole at the bottom of the separation tower (4) is communicated with a feed inlet of the alcohol ether reaction kettle (2);
the discharge port of the top of the separation tower (4) is communicated with the feed port of the light component removal tower (5), and the discharge port of the light component removal tower (5) is communicated with the feed port of the heavy component removal tower (6).
In addition, the invention provides a device for continuously producing dihydric alcohol, which is characterized by comprising a catalyst preparation kettle (1), wherein a discharge hole of the catalyst reaction kettle (1) is communicated with a feed hole of an alcohol ether reaction kettle (2);
the discharge hole of the alcohol ether reaction kettle (2) is communicated with the feed inlet of the gas-liquid separation tank (3), and the gas outlet of the gas-liquid separation tank (3) is communicated with the gas inlet of the alcohol ether reaction kettle (2);
a discharge hole of the gas-liquid separation tank (3) is communicated with a feed inlet of the separation tower (4), and a discharge hole at the bottom of the separation tower (4) is communicated with a feed inlet of the alcohol ether reaction kettle (2);
the discharge port of the top of the separation tower (4) is communicated with the feed port of the light component removal tower (5), and the discharge port of the light component removal tower (5) is communicated with the feed port of the heavy component removal tower (6).
The invention has the beneficial effects that:
the invention not only realizes the continuous production of the dihydric alcohol vinyl ether, but also greatly improves the production efficiency, enables the reaction which takes longer time to be completed in a short time, and simultaneously ensures the stability of the product. Moreover, the catalyst dehydration activation method provided by the invention obviously improves the reaction rate, greatly reduces the occurrence of side reactions and improves the yield.
Drawings
FIG. 1 is a schematic view of a treating apparatus according to the present invention, which is illustrated by taking 1, 4-butanediol as an example in a glycol
1. Catalyst preparation kettle 2, alcohol ether reaction kettle 3, gas-liquid separation tank 4, knockout tower 5, light tower 6, heavy tower.
Detailed Description
The present invention will be further described with reference to the following examples using 1, 4-butanediol as a raw material, wherein the following examples are only illustrative of the preferred embodiments of the present invention and are not intended to limit the present invention in any way, and those skilled in the art may modify the equivalent embodiments using the technical content disclosed above. Any simple modification or equivalent changes made to the following embodiments according to the technical essence of the present invention, without departing from the technical spirit of the present invention, fall within the scope of the present invention.
Example 1
(1) 100g of 1, 4-butanediol and 8g of potassium hydroxide solid are added into a catalyst reaction kettle 1, heated to 130 ℃, reacted for 0.5h and then conveyed to an alcohol ether reaction kettle 2.
(2) Under the condition of stirring, acetylene gas is introduced into the alcohol ether reaction kettle 2, the pressure is controlled to be 0.35Mpa, and the temperature is slowly increased to 140 ℃ to obtain reaction liquid.
(3) The reaction liquid is conveyed to a gas-liquid separation tank 3, the separated gas is conveyed back to the alcohol ether reaction kettle 2, and the separated liquid is conveyed to a separation tower 4.
(4) The bottom material in the separation tower 4 is conveyed back to the alcohol ether reaction kettle 2, and 50g of fresh 1, 4-butanediol is supplemented according to the liquid level of the alcohol ether reaction kettle 2, so that the liquid level of 70-80% is stabilized; the material at the top of the separation tower 4 is conveyed to a lightness-removing tower 5.
(5) The material at the top of the column was treated in a light ends removal column (5) and transferred to a heavy ends removal column (6) to obtain 8.25g of 1, 4-butanediol vinyl ether.
Example 2
(1) 100g of 1, 4-butanediol and 8g of potassium hydroxide solid are added into a catalyst reaction kettle 1, heated to 130 ℃, decompressed to-0.08 mpa, reacted for 0.5h and then conveyed to an alcohol ether reaction kettle 2.
(2) Under the condition of stirring, acetylene gas is introduced into the alcohol ether reaction kettle 2, the pressure is controlled to be 0.35Mpa, and the temperature is slowly increased to 140 ℃ to obtain reaction liquid.
(3) The reaction liquid is conveyed to a gas-liquid separation tank 3, the separated gas is conveyed back to the alcohol ether reaction kettle 2, and the separated liquid is conveyed to a separation tower 4.
(4) The bottom material in the separation tower 4 is conveyed back to the alcohol ether reaction kettle 2, and 50g of fresh 1, 4-butanediol is supplemented according to the liquid level of the alcohol ether reaction kettle 2, so that the liquid level of 70-80% is stabilized; the material at the top of the separation tower 4 is conveyed to a lightness-removing tower 5.
(5) The material at the top of the column is treated by a light component removal column 5 and then is conveyed to a heavy component removal column 6, and 35.23g of 1, 4-butanediol vinyl ether is obtained.
Example 3
(1) 100g of 1, 4-butanediol and 13g of potassium hydroxide solid are added into a catalyst reaction kettle 1, heated to 130 ℃, decompressed to-0.08 mpa, reacted for 0.5h and then conveyed to an alcohol ether reaction kettle 2.
(2) Under the condition of stirring, acetylene gas is introduced into the alcohol ether reaction kettle 2, the pressure is controlled to be 0.35Mpa, and the temperature is slowly increased to 140 ℃ to obtain reaction liquid.
(3) The reaction liquid is conveyed to a gas-liquid separation tank 3, the separated gas is conveyed back to the alcohol ether reaction kettle 2, and the separated liquid is conveyed to a separation tower 4.
(4) The bottom material in the separation tower 4 is conveyed back to the alcohol ether reaction kettle 2, and 50g of fresh 1, 4-butanediol is supplemented according to the liquid level of the alcohol ether reaction kettle 2, so that the liquid level of 70-80% is stabilized; the material at the top of the separation tower 4 is conveyed to a lightness-removing tower 5.
(5) The material at the top of the column was treated in a light ends removal column 5 and then transferred to a heavy ends removal column 6 to obtain 28.49g of 1, 4-butanediol vinyl ether.
Example 4
(1) 100g of 1, 4-butanediol and 4g of potassium hydroxide solid are added into a catalyst reaction kettle 1, heated to 130 ℃, decompressed to-0.08 mpa, reacted for 0.5h and then conveyed to an alcohol ether reaction kettle 2.
(2) Under the condition of stirring, acetylene gas is introduced into the alcohol ether reaction kettle 2, the pressure is controlled to be 0.35Mpa, and the temperature is slowly increased to 140 ℃ to obtain reaction liquid.
(3) The reaction liquid is conveyed to a gas-liquid separation tank 3, the separated gas is conveyed back to the alcohol ether reaction kettle 2, and the separated liquid is conveyed to a separation tower 4.
(4) The bottom material in the separation tower 4 is conveyed back to the alcohol ether reaction kettle 2, and 50g of fresh 1, 4-butanediol is supplemented according to the liquid level of the alcohol ether reaction kettle (2), so that 70-80% of the liquid level is stabilized; the material at the top of the separation tower 4 is conveyed to a lightness-removing tower 5.
(5) The material at the top of the column was treated in a light ends removal column 5 and then transferred to a heavy ends removal column 6 to obtain 21.17g of 1, 4-butanediol vinyl ether.
Example 5
(1) 100g of 1, 4-butanediol and 8g of potassium hydroxide solid are added into a catalyst reaction kettle 1, heated to 130 ℃, decompressed to-0.08 mpa, reacted for 0.5h and then conveyed to an alcohol ether reaction kettle 2.
(2) Under the condition of stirring, acetylene gas is introduced into the alcohol ether reaction kettle 2, the pressure is controlled to be 0.35Mpa, and the temperature is slowly increased to 160 ℃, so as to obtain a reaction solution.
(3) The reaction liquid is conveyed to a gas-liquid separation tank 3, the separated gas is conveyed back to the alcohol ether reaction kettle 2, and the separated liquid is conveyed to a separation tower 4.
(4) The bottom material in the separation tower 4 is conveyed back to the alcohol ether reaction kettle 2, and 50g of fresh 1, 4-butanediol is supplemented according to the liquid level of the alcohol ether reaction kettle 2, so that the liquid level of 70-80% is stabilized; the material at the top of the separation tower 4 is conveyed to a lightness-removing tower 5.
(5) The material at the top of the column is treated by a light component removing column 5 and then is conveyed to a heavy component removing column 6, and 30.68g of 1, 4-butanediol vinyl ether is obtained.
Example 6
(1) 100g of 1, 4-butanediol and 8g of potassium hydroxide solid are added into a catalyst reaction kettle 1, heated to 130 ℃, decompressed to-0.08 mpa, reacted for 0.5h and then conveyed to an alcohol ether reaction kettle 2.
(2) Under the condition of stirring, acetylene gas is introduced into the alcohol ether reaction kettle 2, the pressure is controlled to be 0.35Mpa, and the temperature is slowly increased to 130 ℃, so as to obtain a reaction solution.
(3) The reaction liquid is conveyed to a gas-liquid separation tank 3, the separated gas is conveyed back to the alcohol ether reaction kettle 2, and the separated liquid is conveyed to a separation tower 4.
(4) The bottom material in the separation tower 4 is conveyed back to the alcohol ether reaction kettle 2, and 50g of fresh 1, 4-butanediol is supplemented according to the liquid level of the alcohol ether reaction kettle 2, so that the liquid level of 70-80% is stabilized; the material at the top of the separation tower 4 is conveyed to a lightness-removing tower 5.
(5) The material at the top of the column was treated in a light ends removal column 5 and then transferred to a heavy ends removal column 6 to obtain 31.78g of 1, 4-butanediol vinyl ether.
Example 7
The device for continuously producing the dihydric alcohol comprises a catalyst preparation kettle 1, wherein a discharge hole of the catalyst reaction kettle 1 is communicated with a feed inlet of an alcohol ether reaction kettle 2;
the discharge hole of the alcohol ether reaction kettle 2 is communicated with the feed inlet of the gas-liquid separation tank 3, and the gas outlet of the gas-liquid separation tank 3 is communicated with the gas inlet of the alcohol ether reaction kettle 2;
a discharge hole of the gas-liquid separation tank 3 is communicated with a feed inlet of a separation tower 4, and a discharge hole at the bottom of the separation tower 4 is communicated with a feed inlet of the alcohol ether reaction kettle 2;
the discharge port of the top of the separation tower 4 is communicated with the feed port of the light component removing tower 5, and the discharge port of the light component removing tower 5 is communicated with the feed port of the heavy component removing tower 6.
Claims (8)
1. A continuous production process of dihydric alcohol vinyl ether is characterized by comprising the following steps:
(1) adding potassium hydroxide and dihydric alcohol into a catalyst preparation kettle (1), heating to 50-180 ℃, reducing the pressure to-0.05-0.1 mpa, and reacting for 0.1-2 h to obtain a catalyst;
(2) injecting the catalyst into an alcohol ether reaction kettle (2), introducing acetylene gas into the alcohol ether reaction kettle (2) under the condition of stirring, controlling the pressure to be 0-5mpa, and slowly heating to 80-180 ℃ to obtain a reaction solution;
(3) the reaction liquid is conveyed to a gas-liquid separation tank (3), the separated gas is conveyed back to the alcohol ether reaction kettle (2), and the separated liquid is conveyed to a separation tower (4);
(4) the tower bottom material in the separation tower (4) is conveyed back to the alcohol ether reaction kettle (2), fresh dihydric alcohol is supplemented according to the liquid level of the alcohol ether reaction kettle (2) to stabilize the liquid level at 70-80%, and the tower top material in the separation tower (4) is conveyed to the light component removal tower (5);
(5) and (3) treating the material at the top of the tower by a light component removal tower (5), and conveying the material to a heavy component removal tower (6) to obtain the dihydric alcohol vinyl ether.
2. The process according to claim 1, wherein the diol is one of ethylene glycol, diethylene glycol, and 1, 4-butanediol.
3. The production process according to claim 1, wherein the diol: the ratio of potassium hydroxide is 100: 1-50.
4. The production process according to claim 1, wherein the alcohol ether reaction kettle is a self-suction reaction kettle.
5. The production process according to claim 4, wherein the self-priming reaction kettle is controlled to be constant in liquid level and pressure by the feeding of fresh alcohol and acetylene gas.
6. The production process according to claim 1,
the treatment device of the production process comprises a catalyst preparation kettle (1), wherein a discharge hole of the catalyst reaction kettle (1) is communicated with a feed hole of the alcohol ether reaction kettle (2);
the discharge hole of the alcohol ether reaction kettle (2) is communicated with the feed inlet of the gas-liquid separation tank (3), and the gas outlet of the gas-liquid separation tank (3) is communicated with the gas inlet of the alcohol ether reaction kettle (2);
a discharge hole of the gas-liquid separation tank (3) is communicated with a feed inlet of the separation tower (4), and a discharge hole at the bottom of the separation tower (4) is communicated with a feed inlet of the alcohol ether reaction kettle (2);
the discharge port of the top of the separation tower (4) is communicated with the feed port of the light component removal tower (5), and the discharge port of the light component removal tower (5) is communicated with the feed port of the heavy component removal tower (6).
7. A continuous production process of 1, 4-butanediol vinyl ether is characterized by comprising the following steps:
(1) adding potassium hydroxide and 1, 4-butanediol into a catalyst preparation kettle (1), heating to 130 ℃, reducing the pressure to-0.08 mpampa, and reacting for 0.5h to obtain a catalyst; according to the mass ratio, the ratio of 1, 4-butanediol: potassium hydroxide is 100: 8;
(2) injecting the catalyst into an alcohol ether reaction kettle (2), introducing acetylene gas into the alcohol ether reaction kettle (2) under the condition of stirring, boosting the pressure to 0.35mpa, and slowly heating to 140 ℃ to obtain a reaction solution; the alcohol ether reaction kettle is a self-suction reaction kettle;
(3) the reaction liquid is conveyed to a gas-liquid separation tank (3), the separated gas is conveyed back to the alcohol ether reaction kettle (2), and the separated liquid is conveyed to a separation tower (4);
(4) the tower bottom material in the separation tower (4) is conveyed back to the alcohol ether reaction kettle (2), fresh 1, 4-butanediol is supplemented according to the liquid level of the alcohol ether reaction kettle (2) to stabilize the liquid level at 70% -80%, and the tower top material in the separation tower (4) is conveyed to the light component removal tower (5);
(5) the material at the top of the tower is treated by a light component removing tower (5) and then is conveyed to a heavy component removing tower (6) to obtain 1,4 butanediol vinyl ether;
the treatment device of the production process comprises a catalyst preparation kettle (1), wherein a discharge hole of the catalyst reaction kettle (1) is communicated with a feed hole of the alcohol ether reaction kettle (2);
the discharge hole of the alcohol ether reaction kettle (2) is communicated with the feed inlet of the gas-liquid separation tank (3), and the gas outlet of the gas-liquid separation tank (3) is communicated with the gas inlet of the alcohol ether reaction kettle (2);
a discharge hole of the gas-liquid separation tank (3) is communicated with a feed inlet of the separation tower (4), and a discharge hole at the bottom of the separation tower (4) is communicated with a feed inlet of the alcohol ether reaction kettle (2);
the discharge port of the top of the separation tower (4) is communicated with the feed port of the light component removal tower (5), and the discharge port of the light component removal tower (5) is communicated with the feed port of the heavy component removal tower (6).
8. The device for continuously producing the dihydric alcohol is characterized by comprising a catalyst preparation kettle (1), wherein a discharge hole of the catalyst reaction kettle (1) is communicated with a feed hole of an alcohol ether reaction kettle (2);
the discharge hole of the alcohol ether reaction kettle (2) is communicated with the feed inlet of the gas-liquid separation tank (3), and the gas outlet of the gas-liquid separation tank (3) is communicated with the gas inlet of the alcohol ether reaction kettle (2);
a discharge hole of the gas-liquid separation tank (3) is communicated with a feed inlet of the separation tower (4), and a discharge hole at the bottom of the separation tower (4) is communicated with a feed inlet of the alcohol ether reaction kettle (2);
the discharge port of the top of the separation tower (4) is communicated with the feed port of the light component removal tower (5), and the discharge port of the light component removal tower (5) is communicated with the feed port of the heavy component removal tower (6).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527067A (en) * | 2021-07-08 | 2021-10-22 | 安徽海螺新材料科技有限公司 | Preparation method of initiator for polycarboxylate superplasticizer polyether macromonomer |
| CN114478203A (en) * | 2022-01-28 | 2022-05-13 | 沧州中润化学助剂有限公司 | Preparation method of vinyl low-carbon alcohol for polyether initiator |
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| JP2006008519A (en) * | 2004-06-22 | 2006-01-12 | Maruzen Petrochem Co Ltd | Method for producing triethylene glycol divinyl ether |
| CN102976904A (en) * | 2012-12-24 | 2013-03-20 | 厦门大学 | Preparation device of isobutyl vinyl ether and preparation method thereof |
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|---|---|---|---|---|
| JP2006008519A (en) * | 2004-06-22 | 2006-01-12 | Maruzen Petrochem Co Ltd | Method for producing triethylene glycol divinyl ether |
| CN102976904A (en) * | 2012-12-24 | 2013-03-20 | 厦门大学 | Preparation device of isobutyl vinyl ether and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113527067A (en) * | 2021-07-08 | 2021-10-22 | 安徽海螺新材料科技有限公司 | Preparation method of initiator for polycarboxylate superplasticizer polyether macromonomer |
| CN114478203A (en) * | 2022-01-28 | 2022-05-13 | 沧州中润化学助剂有限公司 | Preparation method of vinyl low-carbon alcohol for polyether initiator |
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