CN220940693U - Esterification reaction device - Google Patents
Esterification reaction device Download PDFInfo
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- CN220940693U CN220940693U CN202322231027.9U CN202322231027U CN220940693U CN 220940693 U CN220940693 U CN 220940693U CN 202322231027 U CN202322231027 U CN 202322231027U CN 220940693 U CN220940693 U CN 220940693U
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- 238000005886 esterification reaction Methods 0.000 title claims abstract description 297
- 230000032050 esterification Effects 0.000 claims abstract description 234
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 60
- 239000002994 raw material Substances 0.000 claims description 60
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 35
- 238000006386 neutralization reaction Methods 0.000 claims description 31
- 239000011552 falling film Substances 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 27
- 239000006096 absorbing agent Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 238000009834 vaporization Methods 0.000 claims description 22
- 230000008016 vaporization Effects 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 16
- 238000003860 storage Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 13
- 238000000746 purification Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- BFHXLRDUQISVTP-UHFFFAOYSA-N Cl[SiH](Cl)Cl.CC Chemical compound Cl[SiH](Cl)Cl.CC BFHXLRDUQISVTP-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000011084 recovery Methods 0.000 claims description 7
- 239000000498 cooling water Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000000047 product Substances 0.000 description 50
- 239000007789 gas Substances 0.000 description 44
- 238000010586 diagram Methods 0.000 description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- LMQGXNPPTQOGDG-UHFFFAOYSA-N trimethoxy(trimethoxysilyl)silane Chemical compound CO[Si](OC)(OC)[Si](OC)(OC)OC LMQGXNPPTQOGDG-UHFFFAOYSA-N 0.000 description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000007273 lactonization reaction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000159 acid neutralizing agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- JCGDCINCKDQXDX-UHFFFAOYSA-N trimethoxy(2-trimethoxysilylethyl)silane Chemical compound CO[Si](OC)(OC)CC[Si](OC)(OC)OC JCGDCINCKDQXDX-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model provides an esterification reaction device, including esterification system, little circulation line, big circulation line, esterification system includes esterification tower, esterification kettle, the bottom of esterification tower and the top intercommunication of esterification kettle, the both ends of little circulation line respectively with the esterification product export of seting up of esterification kettle bottom, the second reflux entry intercommunication of seting up at esterification kettle top, the both ends of big circulation line respectively with the esterification product export, the first reflux entry intercommunication of seting up at esterification tower top, little circulation line, big circulation line are according to the esterification product degree of esterification that esterification product exit obtained and are selected to open or close. The design can switch between a small circulation pipeline and a large circulation pipeline according to the esterification degree of the esterification product, and the preparation efficiency and the economy are considered.
Description
Technical Field
The utility model belongs to the technical field of siloxane preparation equipment, and particularly relates to an esterification reaction device which is suitable for improving the esterification degree and reducing product impurities.
Background
The existing esterification reaction device mostly adopts an esterification tower or an esterification kettle, has a short reaction route and is mainly used for esterification reaction with fewer esterification sites, but for raw materials with more esterification sites, for example, when 1, 2-bis (trichlorosilane) ethane is used as a raw material to prepare hexamethoxy disilyl ethane, six esterification sites on the raw material cannot be completely esterified, and the problem of more impurities of the prepared products exists. Therefore, the prior art has the problems of lower esterification degree of raw materials and more impurities of products.
Disclosure of Invention
The utility model aims to solve the problems in the prior art and provide an esterification reaction device for improving the esterification degree and reducing the impurity of a product.
In order to achieve the above object, the technical scheme of the present utility model is as follows:
The esterification reaction device comprises an esterification system, a small circulation pipeline and a large circulation pipeline, wherein the esterification system comprises an esterification tower and an esterification kettle, the bottom of the esterification tower is communicated with the top of the esterification kettle, the two ends of the small circulation pipeline are respectively communicated with an esterification product outlet formed in the bottom of the esterification kettle and a second backflow inlet formed in the top of the esterification kettle, and the two ends of the large circulation pipeline are respectively communicated with an esterification product outlet and a first backflow inlet formed in the top of the esterification tower;
The small circulation pipeline and the large circulation pipeline are selectively opened or closed according to the esterification degree of the esterification product obtained at the esterification product outlet.
When the esterification degree of the esterification product is high, the small circulation pipeline is opened, and the large circulation pipeline is closed;
when the esterification degree of the esterification product is low, the small circulation pipeline is closed, and the large circulation pipeline is opened.
The top of the esterification tower is also provided with a pre-esterification mixed liquid inlet, and the top of the esterification kettle is also provided with a steam inlet;
The esterification tower is used for carrying out esterification reaction on pre-esterification mixed liquor and steam formed by vaporization of carboxylic acid raw materials to generate esterification liquor, and the pre-esterification mixed liquor is obtained by carrying out esterification reaction on the carboxylic acid raw materials and alcohol raw materials;
the esterification kettle is used for allowing esterification liquid from the esterification tower to generate an esterification product.
The carboxylic acid raw material is methanol, and the alcohol raw material is-bis (trichlorosilane) ethane.
The esterification system further comprises a vaporization kettle, a buffer tank and a mixing tank, wherein a first carboxylic acid raw material inlet is arranged on the vaporization kettle, an outlet of the vaporization kettle is communicated with an inlet of the buffer tank, an outlet of the buffer tank is communicated with a steam inlet, a second carboxylic acid raw material inlet and an alcohol raw material inlet are arranged on the mixing tank, and two overflow ports of the mixing tank are communicated with a pre-esterification mixed liquid inlet;
The esterification reaction device also comprises a neutralization system and a filtration purification system, wherein the inlet of the neutralization system is communicated with the esterification product outlet, the outlet of the neutralization system is communicated with the inlet of the filtration purification system, and the outlet of the filtration purification system is communicated with the storage tank.
The neutralization system comprises a neutralization kettle, the filtration purification system comprises a microporous filter and a rectifying tower kettle, an inlet of the neutralization kettle is communicated with an esterification product outlet, an outlet of the neutralization kettle is communicated with an inlet of the microporous filter, an outlet of the microporous filter is communicated with an inlet of the rectifying tower kettle, and an outlet of the rectifying tower kettle is communicated with a storage tank.
The esterification reaction device further comprises a circulating recovery system, the circulating recovery system comprises a water cooler and a condenser, a first gas inlet of the water cooler is communicated with a first mixed gas outlet formed in the top of the esterification tower and a second mixed gas outlet formed in the top of the mixing tank, a first gas outlet of the water cooler is communicated with a second gas inlet of the condenser, and a first cooling product outlet of the water cooler and a second cooling product outlet of the condenser are both used for outputting carboxylic acid raw materials obtained through separation.
The water cooler and the hydraulic condenser are both used for cooling mixed gas from the esterification tower and the mixing tank, and the mixed gas is acid gas with carboxylic acid raw materials.
The esterification reaction device further comprises an acid making system, the acid making system comprises a falling film absorber, an inlet of the falling film absorber is communicated with a second gas outlet of the condenser, an outlet of the falling film absorber is communicated with a hydrochloric acid storage tank, and a circulating cooling water system for absorbing reaction heat of the falling film absorber is arranged outside the falling film absorber.
The inside axial of esterifying the cauldron is provided with the material agitator, and the outside of esterifying the cauldron is provided with the cauldron jacket that is used for heating the material in the cauldron.
Compared with the prior art, the utility model has the beneficial effects that:
1. The utility model relates to an esterification reaction device, which comprises an esterification system, a small circulation pipeline and a large circulation pipeline, wherein the esterification system comprises an esterification tower and an esterification kettle, the bottom of the esterification tower is communicated with the top of the esterification kettle, two ends of the small circulation pipeline are respectively communicated with an esterification product outlet formed in the bottom of the esterification kettle and a second backflow inlet formed in the top of the esterification kettle, two ends of the large circulation pipeline are respectively communicated with the esterification product outlet and a first backflow inlet formed in the top of the esterification tower, and the small circulation pipeline and the large circulation pipeline are selectively opened or closed according to the esterification degree of an esterification product obtained at the esterification product outlet; the design can be switched between a small circulation pipeline and a large circulation pipeline according to the esterification degree of the esterification product, so that the esterification degree is improved, and the impurity of the product is reduced. Therefore, the utility model can improve the esterification degree and reduce the impurity of the product.
2. In the esterification reaction device, when the esterification degree of an esterification product is high, a small circulation pipeline is opened, a large circulation pipeline is closed, and when the esterification degree of the esterification product is low, the small circulation pipeline is closed, and the large circulation pipeline is opened; the design uses a large circulation pipeline with a longer reaction line when the esterification degree of an esterification product is low, ensures higher reaction efficiency, and uses a small circulation pipeline with a shorter reaction line after the esterification degree of the esterification product is improved, so that the energy consumption of the whole preparation process is controlled in a proper range. Therefore, the utility model not only can ensure higher reaction efficiency, but also can ensure the energy consumption of the whole preparation process to be in a proper range.
3. In the esterification reaction device, the top of an esterification tower is also provided with a pre-esterification mixed liquid inlet, the top of an esterification kettle is also provided with a steam inlet, the esterification tower is used for carrying out esterification reaction on the pre-esterification mixed liquid and steam formed by vaporization of carboxylic acid raw materials to generate esterification liquid, the esterification kettle is used for carrying out esterification reaction on the esterification liquid from the esterification tower to generate esterification products, and the pre-esterification mixed liquid is obtained by carrying out esterification reaction on the carboxylic acid raw materials and alcohol raw materials; because the alcohol raw material is solid at normal temperature, in the design, the alcohol raw material and part of carboxylic acid raw material are firstly mixed, a small part of esterification sites on the alcohol raw material are subjected to esterification reaction, and then the solid state is converted into liquid pre-esterification mixed liquid, and then the pre-esterification mixed liquid is input into an esterification tower to be mixed with steam formed by the vaporization of the carboxylic acid raw material, so that the two raw materials are fully mixed, the esterification reaction efficiency can be improved, and the whole preparation time is shortened. Therefore, the utility model can improve the esterification reaction efficiency and shorten the whole preparation time.
4. In the esterification reaction device, a material stirrer is axially arranged in an esterification kettle, and a kettle jacket for heating materials in the kettle is arranged outside the esterification kettle; in the design, the esterification reaction of the esterification liquid in the esterification kettle is completed under the heating of steam of a kettle jacket, and the materials in the esterification kettle are stirred by a material stirrer in the process, so that the esterification reaction efficiency is further improved. Therefore, the present utility model can further improve the esterification reaction efficiency.
Drawings
FIG. 1 is a schematic diagram of the structure of an esterification system according to the present utility model.
FIG. 2 is a schematic diagram of the structure of the esterification tower and the esterification kettle in the utility model.
Fig. 3 is a schematic structural view of a mixing tank in the utility model.
FIG. 4 is a schematic diagram of the recycling system according to the present utility model.
Fig. 5 is a schematic structural view of a buffer tank according to the present utility model.
FIG. 6 is a schematic diagram of a vaporization kettle in accordance with the present utility model.
FIG. 7 is a schematic diagram of the structure of the neutralization tank in the present utility model.
FIG. 8 is a schematic diagram of a filtration purification system according to the present utility model.
FIG. 9 is a schematic diagram of an acid making system according to the present utility model.
In the above figure, the esterification system 1, the esterification column 11, the pre-esterification mixed liquor inlet 111, the first reflux inlet 112, the steam inlet 113, the first mixed gas outlet 114, the carboxylic acid raw material reflux inlet 115, the esterification reactor 12, the second reflux inlet 121, the esterification product outlet 122, the material stirrer 123, the vaporization reactor 13, the first carboxylic acid raw material inlet 131, the buffer tank 14, the mixing tank 15, the second carboxylic acid raw material inlet 151, the alcohol raw material inlet 152, the second mixed gas outlet 153, the overflow port 154, the small circulation line 21, the large circulation line 22, the neutralization system 3, the neutralization reactor 31, the filtration and purification system 4, the microporous filter 41, the rectification column reactor 42, the circulation recovery system 5, the water cooler 51, the first gas inlet 511, the first gas outlet 512, the first cooling product outlet 513, the condenser 52, the second gas inlet 521, the second cooling product outlet 522, the second gas outlet 523, the acid production system 6, and the falling film absorber 61 are shown.
Detailed Description
The present utility model will be described in further detail with reference to the following detailed description and the accompanying drawings.
Referring to fig. 1 to 9, an esterification reaction device comprises an esterification system 1, a small circulation pipeline 21 and a large circulation pipeline 22, wherein the esterification system 1 comprises an esterification tower 11 and an esterification kettle 12, the bottom of the esterification tower 11 is communicated with the top of the esterification kettle 12, two ends of the small circulation pipeline 21 are respectively communicated with an esterification product outlet 122 formed in the bottom of the esterification kettle 12 and a second reflux inlet 121 formed in the top of the esterification kettle 12, and two ends of the large circulation pipeline 22 are respectively communicated with the esterification product outlet 122 and a first reflux inlet 112 formed in the top of the esterification tower 11;
the small circulation line 21 and the large circulation line 22 are selectively opened or closed according to the esterification degree of the esterification product obtained at the esterification product outlet 122.
When the esterification degree of the esterification product is high, the small circulation pipeline 21 is opened, and the large circulation pipeline 22 is closed;
when the esterification degree of the esterification product is low, the small circulation line 21 is closed and the large circulation line 22 is opened.
The top of the esterification tower 11 is also provided with a pre-esterification mixed liquid inlet 111, and the top of the esterification kettle 12 is also provided with a steam inlet 113;
The esterification tower 11 is used for carrying out esterification reaction on pre-esterification mixed liquor and steam formed by vaporization of carboxylic acid raw materials to generate esterification liquor, wherein the pre-esterification mixed liquor is obtained by carrying out esterification reaction on the carboxylic acid raw materials and alcohol raw materials;
the esterification kettle 12 is used for allowing the esterification liquid from the esterification tower 11 to generate an esterification product.
The carboxylic acid raw material is methanol, and the alcohol raw material is 1, 2-bis (trichlorosilane) ethane.
The esterification system 1 further comprises a vaporization kettle 13, a buffer tank 14 and a mixing tank 15, wherein a first carboxylic acid raw material inlet 131 is arranged on the vaporization kettle 13, an outlet of the vaporization kettle 13 is communicated with an inlet of the buffer tank 14, an outlet of the buffer tank 14 is communicated with a steam inlet 113, a second carboxylic acid raw material inlet 151 and an alcohol raw material inlet 152 are arranged on the mixing tank 15, and two overflow ports 154 of the mixing tank 15 are both communicated with a pre-esterification mixed liquid inlet 111;
the esterification reaction device also comprises a neutralization system 3 and a filtration purification system 4, wherein the inlet of the neutralization system 3 is communicated with an esterification product outlet 122, the outlet of the neutralization system 3 is communicated with the inlet of the filtration purification system 4, and the outlet of the filtration purification system 4 is communicated with a storage tank.
The neutralization system 3 comprises a neutralization kettle 31, the filtering and purifying system 4 comprises a microporous filter 41 and a rectifying tower kettle 42, an inlet of the neutralization kettle 31 is communicated with an esterification product outlet 122, an outlet of the neutralization kettle 31 is communicated with an inlet of the microporous filter 41, an outlet of the microporous filter 41 is communicated with an inlet of the rectifying tower kettle 42, and an outlet of the rectifying tower kettle 42 is communicated with a storage tank.
The esterification reaction device further comprises a recycling system 5, the recycling system 5 comprises a water cooler 51 and a condenser 52, a first gas inlet 511 of the water cooler 51 is communicated with a first mixed gas outlet 114 formed in the top of the esterification tower 11 and a second mixed gas outlet 153 formed in the top of the mixing tank 15, a first gas outlet 512 of the water cooler 51 is communicated with a second gas inlet 521 of the condenser 52, and a first cooling product outlet 513 of the water cooler 51 and a second cooling product outlet 522 of the condenser 52 are both used for outputting separated carboxylic acid raw materials;
The water cooler 51 and the hydraulic condenser are used for cooling the mixed gas from the esterification tower 11 and the mixing tank 15, wherein the mixed gas is acid gas with carboxylic acid raw materials.
The esterification reaction device further comprises an acid making system 6, the acid making system 6 comprises a falling film absorber 61, an inlet of the falling film absorber 61 is communicated with a second gas outlet 523 of the condenser 52, an outlet of the falling film absorber 61 is communicated with a hydrochloric acid storage tank, and a circulating cooling water system for absorbing reaction heat of the falling film absorber 61 is arranged outside the falling film absorber 61.
The inside axial of esterifying cauldron 12 is provided with material agitator 123, and the outside of esterifying cauldron 12 is provided with the cauldron jacket that is used for heating the material in the cauldron.
The principle of the utility model is explained as follows:
The esterification reaction device is suitable for preparing the hexamethoxy disilane by taking methanol and 1, 2-bis (trichlorosilane) ethane as raw materials, wherein when 1-3 chlorine on the 1, 2-bis (trichlorosilane) ethane participates in the esterification reaction and is replaced by methyl, the esterification degree is low, and when at least 4 or 5 chlorine participates in the esterification reaction and is replaced by methyl, the esterification degree is high;
The preparation process comprises the following steps:
The anhydrous methanol from the methanol raw material storage tank is firstly conveyed to a methanol metering tank through a shielding pump, and then sequentially conveyed to a vaporization kettle 13 and a mixing tank 15 after passing through a regulating valve and a flowmeter;
The methanol in the vaporization kettle 13 is vaporized under the action of steam, the methanol steam is further heated by the buffer tank 14, and the overheated methanol steam is continuously added to the top of the esterification kettle 12 after passing through the regulating valve and the flowmeter in sequence, and then rises from the top of the esterification kettle 12 to enter the bottom of the esterification tower 11;
1, 2-bis (trichlorosilane) ethane from a 1, 2-bis (trichlorosilane) ethane raw material storage tank is firstly conveyed to a 1, 2-bis (trichlorosilane) ethane metering tank through a shielding pump, then is continuously added into a mixing tank 15 after being controlled by a regulating valve and a flowmeter in sequence, and is subjected to pre-esterification reaction with methanol which is simultaneously added into the mixing tank 15 at the temperature of 40 ℃,1 or 2 chlorine on the 1, 2-bis (trichlorosilane) ethane is replaced by methyl, and a generated pre-esterification mixed solution continuously flows into the top of an esterification tower 11 through an overflow port 154 of the mixing tank 15;
The superheated methanol vapor in the esterification tower 11 is fully contacted with the pre-esterification mixed liquid from the mixing tank 15 on the surface of the filler in the esterification tower 11, and further esterification reaction is carried out, and the generated esterification liquid falls into the esterification kettle 12 under the action of gravity;
The esterification liquid in the esterification kettle 12 is heated to 80-90 ℃ in the steam of the kettle jacket to finish the deep esterification reaction at high temperature, and the byproduct hydrogen chloride gas and excessive methanol of the esterification reaction are further removed from the esterification liquid along with the temperature rise of the kettle lactonization liquid, and the kettle lactonization liquid is transferred into a neutralization kettle 31 after the esterification is completed;
The esterification liquid in the neutralization kettle 31 is subjected to desorption under the conditions of stirring and deep vacuum, methanol, chlorobenzene and hydrogen chloride gas are further removed, the esterification liquid after the desorption treatment is neutralized by a neutralizing agent, the neutralization agent is filtered by a microporous filter 41 to obtain a crude product of the hexamethoxy disilane, the crude product of the hexamethoxy disilane is sent to a rectifying tower kettle 42, and high-purity finished products of the hexamethoxy disilane are obtained by removing high-boiling substances and low-boiling substances through distillation;
The mixed gas of hydrogen chloride and methanol is input into a recycling system 5, the entrained methanol is condensed, the recycled methanol is measured by a flowmeter and returns to the esterification tower 11 for recycling by means of a level difference, the purified hydrogen chloride gas is pumped to a falling film absorber 61 and is subjected to film absorption with dilute acid from a tail gas tower in a falling film pipe of the falling film absorber 61 to prepare 30-31% hydrochloric acid, the outside of the falling film pipe adopts a circulating cooling water system to absorb reaction heat, finished acid is discharged to a hydrochloric acid storage tank from the bottom of the falling film absorber 61, tail gas after the falling film absorption enters the tail gas tower and is subjected to reverse absorption reaction with absorption water from an acid water tank on the surface of a filler in the tail gas tower.
Example 1:
Referring to fig. 1, an esterification reaction device comprises an esterification system 1, a small circulation pipeline 21 and a large circulation pipeline 22, wherein the esterification system 1 comprises an esterification tower 11, an esterification kettle 12, a vaporization kettle 13, a buffer tank 14 and a mixing tank 15, a first carboxylic acid raw material inlet 131 is arranged on the vaporization kettle 13, an outlet of the vaporization kettle 13 is communicated with an inlet of the buffer tank 14, an outlet of the buffer tank 14 is communicated with a steam inlet 113 arranged at the top of the esterification kettle 12, a second carboxylic acid raw material inlet 151 and an alcohol raw material inlet 152 are arranged on the mixing tank 15, two overflow ports 154 of the mixing tank 15 are communicated with a pre-esterification mixed liquid inlet 111 arranged at the top of the esterification tower 11, the bottom of the esterification tower 11 is communicated with the top of the esterification kettle 12, a material stirrer 123 is axially arranged in the esterification kettle 12, two ends of the small circulation pipeline 21 are respectively communicated with an esterification product outlet 122 arranged at the bottom of the esterification kettle 12 and a second reflux inlet 121 arranged at the top of the esterification kettle 12, and two overflow ports 154 of the large circulation pipeline 22 are respectively communicated with the top of the esterification tower 11 and the first reflux inlet 112;
The esterification reaction device takes methanol as carboxylic acid raw materials, takes 1, 2-bis (trichlorosilane) ethane as alcohol raw materials, prepares hexamethoxydisilane, and forms superheated steam after a part of carboxylic acid raw materials sequentially pass through the vaporization kettle 13 and the buffer tank 14, and the other part of carboxylic acid raw materials and alcohol raw materials undergo pre-esterification reaction in the mixing tank 15 to obtain pre-esterification mixed liquor, the pre-esterification mixed liquor enters the esterification tower 11 to undergo esterification reaction with the superheated steam to generate esterification liquor, the esterification liquor falls into the esterification kettle 12, further undergoes esterification reaction at high temperature, the esterification degree of an esterification product obtained at an esterification product outlet 122 of the esterification kettle 12 is detected, if the esterification degree is low, the small circulation pipeline 21 is controlled to be closed, the large circulation pipeline 22 is controlled to be opened, and if the esterification degree is high, the small circulation pipeline 21 is controlled to be closed, and the energy consumption is further reduced while the esterification degree is further improved.
Example 2:
The difference from example 1 is that:
The esterification reaction device further comprises a neutralization system 3 and a filtering and purifying system 4, the neutralization system 3 comprises a neutralization kettle 31, the filtering and purifying system 4 comprises a microporous filter 41 and a rectifying tower kettle 42, an inlet of the neutralization kettle 31 is communicated with an esterification product outlet 122, an outlet of the neutralization kettle 31 is communicated with an inlet of the microporous filter 41, an outlet of the microporous filter 41 is communicated with an inlet of the rectifying tower kettle 42, and an outlet of the rectifying tower kettle 42 is communicated with a storage tank for storing a product finished product.
Example 3:
The difference from example 1 is that:
The esterification reaction device further comprises a circulation recovery system 5 and an acid making system 6, the circulation recovery system 5 comprises a water cooler 51 and a condenser 52, the acid making system 6 comprises a falling film absorber 61, a first gas inlet 511 of the water cooler 51 is communicated with a first mixed gas outlet 114 formed in the top of the esterification tower 11 and a second mixed gas outlet 153 formed in the top of the mixing tank 15, a first gas outlet 512 of the water cooler 51 is communicated with a second gas inlet 521 of the condenser 52, a first cooling product outlet 513 of the water cooler 51 and a second cooling product outlet 522 of the condenser 52 are both used for outputting separated carboxylic acid raw materials, the recovered carboxylic acid raw materials can be input into the esterification tower 11 to participate in esterification reaction, an inlet of the falling film absorber 61 is communicated with a second gas outlet 523 of the condenser 52, an outlet of the falling film absorber 61 is communicated with a hydrochloric acid storage tank, and a circulation cooling water system for absorbing reaction heat of the falling film absorber 61 is arranged outside the falling film absorber 61;
The mixed gas from the esterification tower 11 and the mixing tank 15 is cooled by a water cooler 51 and a hydraulic condenser, the mixed gas is hydrogen chloride gas with methanol, the methanol is condensed, the mixed gas is measured by a flowmeter, the mixed gas returns to the esterification tower 11 by the potential difference for recycling, and the purified hydrogen chloride gas enters a falling film absorber 61 for film absorption to prepare 30-31% hydrochloric acid and is discharged to a hydrochloric acid storage tank.
Claims (10)
1. An esterification reaction apparatus, characterized in that:
The esterification reaction device comprises an esterification system (1), a small circulation pipeline (21) and a large circulation pipeline (22), wherein the esterification system (1) comprises an esterification tower (11) and an esterification kettle (12), the bottom of the esterification tower (11) is communicated with the top of the esterification kettle (12), two ends of the small circulation pipeline (21) are respectively communicated with an esterification product outlet (122) formed in the bottom of the esterification kettle (12) and a second backflow inlet (121) formed in the top of the esterification kettle (12), and two ends of the large circulation pipeline (22) are respectively communicated with the esterification product outlet (122) and a first backflow inlet (112) formed in the top of the esterification tower (11);
The small circulation pipeline (21) and the large circulation pipeline (22) are selectively opened or closed according to the esterification degree of the esterification product obtained at the esterification product outlet (122).
2. An esterification reaction apparatus according to claim 1, characterized in that:
When the esterification degree of the esterification product is high, the small circulation pipeline (21) is opened, and the large circulation pipeline (22) is closed;
when the esterification degree of the esterification product is low, the small circulation pipeline (21) is closed, and the large circulation pipeline (22) is opened.
3. An esterification reaction apparatus according to claim 1 or 2, characterized in that:
The top of the esterification tower (11) is also provided with a pre-esterification mixed liquid inlet (111), and the top of the esterification kettle (12) is also provided with a steam inlet (113);
The esterification tower (11) is used for carrying out esterification reaction on pre-esterification mixed liquor and steam formed by vaporization of carboxylic acid raw materials to generate esterification liquor, and the pre-esterification mixed liquor is obtained by carrying out esterification reaction on the carboxylic acid raw materials and alcohol raw materials;
The esterification kettle (12) is used for allowing the esterification liquid from the esterification tower (11) to generate an esterification product.
4. An esterification reaction apparatus according to claim 3, characterized in that:
the carboxylic acid raw material is methanol, and the alcohol raw material is 1, 2-bis (trichlorosilane) ethane.
5. An esterification reaction apparatus according to claim 3, characterized in that:
The esterification system (1) further comprises a vaporization kettle (13), a buffer tank (14) and a mixing tank (15), wherein a first carboxylic acid raw material inlet (131) is formed in the vaporization kettle (13), an outlet of the vaporization kettle (13) is communicated with an inlet of the buffer tank (14), an outlet of the buffer tank (14) is communicated with a steam inlet (113), a second carboxylic acid raw material inlet (151) and an alcohol raw material inlet (152) are formed in the mixing tank (15), and two overflow ports (154) of the mixing tank (15) are communicated with a pre-esterification mixed liquid inlet (111).
6. An esterification reaction apparatus according to claim 3, characterized in that:
the esterification reaction device further comprises a neutralization system (3) and a filtering purification system (4), wherein the inlet of the neutralization system (3) is communicated with an esterification product outlet (122), the outlet of the neutralization system (3) is communicated with the inlet of the filtering purification system (4), and the outlet of the filtering purification system (4) is communicated with a storage tank.
7. An esterification reaction apparatus according to claim 6, wherein:
the neutralization system (3) comprises a neutralization kettle (31), the filtration purification system (4) comprises a microporous filter (41) and a rectifying tower kettle (42), an inlet of the neutralization kettle (31) is communicated with an esterification product outlet (122), an outlet of the neutralization kettle (31) is communicated with an inlet of the microporous filter (41), an outlet of the microporous filter (41) is communicated with an inlet of the rectifying tower kettle (42), and an outlet of the rectifying tower kettle (42) is communicated with a storage tank.
8. An esterification reaction apparatus according to claim 3, characterized in that:
The esterification reaction device further comprises a circulating recovery system (5), the circulating recovery system (5) comprises a water cooler (51) and a condenser (52), a first gas inlet (511) of the water cooler (51) is communicated with a first mixed gas outlet (114) formed in the top of the esterification tower (11) and a second mixed gas outlet (153) formed in the top of the mixing tank (15), a first gas outlet (512) of the water cooler (51) is communicated with a second gas inlet (521) of the condenser (52), and a first cooling product outlet (513) of the water cooler (51) and a second cooling product outlet (522) of the condenser (52) are both used for outputting separated carboxylic acid raw materials;
The water cooler (51) and the hydraulic condenser are both used for cooling mixed gas from the esterification tower (11) and the mixing tank (15), and the mixed gas is acid gas with carboxylic acid raw materials.
9. An esterification reaction apparatus according to claim 8, wherein:
The esterification reaction device further comprises an acid making system (6), the acid making system (6) comprises a falling film absorber (61), an inlet of the falling film absorber (61) is communicated with a second gas outlet (523) of the condenser (52), an outlet of the falling film absorber (61) is communicated with a hydrochloric acid storage tank, and a circulating cooling water system for absorbing reaction heat of the falling film absorber (61) is arranged outside the falling film absorber (61).
10. An esterification reaction apparatus according to claim 1 or 2, characterized in that:
The inside axial of esterifying cauldron (12) is provided with material agitator (123), and the outside of esterifying cauldron (12) is provided with the cauldron jacket that is used for heating the material in the cauldron.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202322231027.9U CN220940693U (en) | 2023-08-18 | 2023-08-18 | Esterification reaction device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202322231027.9U CN220940693U (en) | 2023-08-18 | 2023-08-18 | Esterification reaction device |
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