CN110183479B - System and process for hydrolyzing low-pressure dimethyldichlorosilane - Google Patents
System and process for hydrolyzing low-pressure dimethyldichlorosilane Download PDFInfo
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- CN110183479B CN110183479B CN201910522412.4A CN201910522412A CN110183479B CN 110183479 B CN110183479 B CN 110183479B CN 201910522412 A CN201910522412 A CN 201910522412A CN 110183479 B CN110183479 B CN 110183479B
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- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims description 44
- 230000008569 process Effects 0.000 title claims description 39
- 230000003301 hydrolyzing effect Effects 0.000 title claims description 16
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 69
- 230000007062 hydrolysis Effects 0.000 claims abstract description 52
- 239000012071 phase Substances 0.000 claims abstract description 40
- 239000010408 film Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000009826 distribution Methods 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000007791 liquid phase Substances 0.000 claims abstract description 13
- 239000011552 falling film Substances 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 79
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 33
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 33
- 239000007789 gas Substances 0.000 claims description 32
- 238000000746 purification Methods 0.000 claims description 19
- 238000003795 desorption Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 10
- 239000011344 liquid material Substances 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000003595 mist Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000000413 hydrolysate Substances 0.000 description 22
- 239000000047 product Substances 0.000 description 19
- 238000005903 acid hydrolysis reaction Methods 0.000 description 10
- 229920006395 saturated elastomer Polymers 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000007795 chemical reaction product Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0836—Compounds with one or more Si-OH or Si-O-metal linkage
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- Chemical & Material Sciences (AREA)
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Abstract
The system comprises a hydrolysis reactor, a circulating pump, an analysis tower and a separator, wherein an outlet of the hydrolysis reactor is connected with an inlet of the analysis tower, a liquid phase outlet of the analysis tower is connected with an inlet of the separator, a water phase outlet of the separator is connected with an inlet of the circulating pump, an outlet of the circulating pump is connected with an inlet of the hydrolysis reactor, and a pipeline between the circulating pump and the hydrolysis reactor is connected with a conveying pipeline of dimethyldichlorosilane; the analysis tower comprises a distribution disc and a film forming assembly, the distribution disc is arranged at the middle-upper part in the falling film analysis tower, liquid distribution holes are formed in the distribution disc, the film forming assembly is arranged below the distribution disc, and the film forming assembly is formed by combining a plurality of groups of herringbone plates; the separator is a vertically arranged cylindrical structure, the bottom of the separator is provided with a water phase outlet, and the top of the separator is provided with an oil phase outlet.
Description
Technical Field
The disclosure relates to a system and a process for low-pressure dimethyldichlorosilane hydrolysis.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
At present, two kinds of dimethyl dichlorosilane hydrolysis processes exist in the industry at home, one of the two kinds of processes is constant boiling acid hydrolysis, the quality of hydrolysate obtained by the process method is relatively good, but the energy consumption is large, the byproduct oil-containing waste acid is difficult to treat, and the process method is not adopted in the industry basically. The other method is saturated acid hydrolysis (often called concentrated acid hydrolysis), and the inventor of the present disclosure finds that the method has the conditions of incomplete reaction of dimethyldichlorosilane, high content of terminal chlorine, high viscosity of hydrolysate and high acid value due to relatively high reaction pressure and relatively high acid concentration, so that the subsequent purification and washing system is relatively complex in arrangement, relatively long in flow, and increases investment and operation cost.
Disclosure of Invention
In order to solve the defects of the prior art, the disclosure aims to provide a system and a process for hydrolyzing low-pressure dimethyldichlorosilane, and the process can obtain hydrolysate products with better quality; meanwhile, the oil content carried by the produced hydrogen chloride gas is greatly reduced, and the influence on a subsequent system is reduced. As the hydrolysis reaction pressure is reduced, the whole load of system equipment and pipelines is reduced, the material circulation is reduced, and the construction cost and the operation cost are reduced to a great extent.
In order to achieve the purpose, the technical scheme of the disclosure is as follows:
on one hand, the system for hydrolyzing the low-pressure dimethyldichlorosilane comprises a hydrolysis reactor, a circulating pump, a desorption tower and a separator, wherein an outlet of the hydrolysis reactor is connected with an inlet of the desorption tower, a liquid-phase outlet of the desorption tower is connected with an inlet of the separator, a water-phase outlet of the separator is connected with an inlet of the circulating pump, an outlet of the circulating pump is connected with an inlet of the hydrolysis reactor, and a pipeline between the circulating pump and the hydrolysis reactor is connected with a conveying pipeline of the dimethyldichlorosilane;
the analysis tower comprises a distribution disc and a film forming component, the distribution disc is arranged at the middle-upper part in the falling film analysis tower, liquid distribution holes are formed in the distribution disc, the film forming component is arranged below the distribution disc, the film forming component is formed by combining a plurality of groups of herringbone plates, a gas phase outlet is formed in the top of the analysis tower, and a liquid phase outlet is formed in the bottom of the analysis tower;
the separator is a vertically arranged cylindrical structure, the bottom of the separator is provided with a water phase outlet, and the top of the separator is provided with an oil phase outlet.
First, the present disclosure provides a circulation pump between the hydrolysis reactor and the separator, and the circulation pump is used for conveying hydrochloric acid in the separator to the hydrolysis reactor, and the circulation pump is used for: 1. and 2, sufficiently premixing the circulating acid and supplemented reaction water to provide water required by the reaction for the hydrolysis reaction of the dimethyldichlorosilane.
Secondly, this disclosure sets up the analytic tower, and the material after the hydrolysis reaction flows into the membrane module of "people" style of calligraphy board combination after entering the analytic tower and makes the hydrogen chloride gas that produces in time escape, has prevented that the gas film from forming, is favorable to hydrolysis reaction forward going more to further improve the reaction yield of product.
Third, this disclosure sets up the circulating pump at hydrolysis reactor import, sets up the analysis tower at hydrolysis reactor export, and this combination setting can make dimethyldichlorosilane reaction more complete, effectively increases dimethyldichlorosilane's conversion rate, makes the acidity value greatly reduced of product moreover, and its acidity value is less than 1.2% (ordinary saturated acid hydrolysis product's acidity value is generally more than 3%).
On the other hand, the low-pressure dimethyl dichlorosilane hydrolysis process is characterized in that the system is provided, hydrochloric acid in a separator is pumped out by a circulating pump, the hydrochloric acid and dimethyl dichlorosilane are premixed and then conveyed to a hydrolysis reactor for primary hydrolysis reaction, a material after the hydrolysis reaction enters an analytical tower, the material forms a liquid film in a film forming component of the analytical tower, hydrogen chloride in the liquid film is separated out and then subjected to secondary hydrolysis reaction, a liquid material after the reaction in the analytical tower enters the separator, the liquid material of the separator is divided into two layers, the lower layer is a water phase layer, the upper layer is an oil phase layer, the water phase layer is hydrochloric acid, the oil phase layer is a product, the reaction pressure is controlled to be below 50kPa, and the temperatures of the hydrolysis reactor and the analytical tower are controlled to be 30-50 ℃.
Through practical industrial verification, the process disclosed by the invention can not only reduce the reaction pressure, but also greatly improve the product yield, wherein the yield is higher than 99.9%, and simultaneously, the acidity value of the product can be greatly reduced, so that the acidity value of the first-stage reaction hydrolysate is below 1.2%.
The beneficial effect of this disclosure does:
1. the system and the process disclosed by the invention have the advantages that the obtained hydrolysate has uniform chain length, more centralized product types, less impurities and better quality.
2. The system and the process can remove the hydrogen chloride gas in time, are beneficial to the hydrolysis reaction of the dimethyldichlorosilane, ensure that the reaction is more complete and the conversion yield is increased. At the same time, the hydrolysate has reduced chloride ions (especially the content of the end group chlorine), so that the acidity value of the product is controlled to be greatly lower than that of the traditional saturated acid hydrolysis product.
3. The process shortens the flow of a hydrolysate purification and washing system, and greatly reduces the load and energy consumption of the subsequent cracking process.
4. The product yield of the disclosed process is higher than 99.9%, and the amount of raw material dimethyldichlorosilane consumed per ton of product hydrolysate is already close to the theoretical value.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure, illustrate embodiments of the disclosure and together with the description serve to explain the disclosure and are not to limit the disclosure.
FIG. 1 is a schematic diagram of the configuration of a system for low pressure dimethyldichlorosilane hydrolysis of example 1 of the present disclosure;
the system comprises a circulating pump 1, a hydrolysis reactor 2, a resolving tower 3, a condenser 4, a dryer 5, a demister 6, a separator 7, a separator 8 and a compressor pump.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. 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 disclosure belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In view of the defects of incomplete reaction of dimethyldichlorosilane, high content of end group chlorine, high viscosity of hydrolysate, high acid value and the like existing in the existing saturated acid hydrolysis, the disclosure provides a system and a process for hydrolyzing low-pressure dimethyldichlorosilane.
In a typical embodiment of the present disclosure, a system for hydrolyzing low-pressure dimethyldichlorosilane is provided, which includes a hydrolysis reactor, a circulation pump, a desorption tower, and a separator, wherein an outlet of the hydrolysis reactor is connected to an inlet of the desorption tower, a liquid phase outlet of the desorption tower is connected to an inlet of the separator, a water phase outlet of the separator is connected to an inlet of the circulation pump, an outlet of the circulation pump is connected to an inlet of the hydrolysis reactor, and a pipeline between the circulation pump and the hydrolysis reactor is connected to a conveying pipeline of dimethyldichlorosilane;
the analysis tower comprises a distribution disc and a film forming assembly, the distribution disc is arranged at the middle-upper part in the falling film analysis tower, liquid distribution holes are formed in the distribution disc, the film forming assembly is arranged below the distribution disc, and the film forming assembly is formed by combining a plurality of groups of herringbone plates;
the separator is a vertically arranged cylindrical structure, the bottom of the separator is provided with a water phase outlet, and the top of the separator is provided with an oil phase outlet.
First, the present disclosure provides a circulation pump between the hydrolysis reactor and the separator, and the circulation pump is used for conveying hydrochloric acid in the separator to the hydrolysis reactor, and the circulation pump is used for: 1. and 2, sufficiently premixing the circulating acid and supplemented reaction water to provide water required by the reaction for the hydrolysis reaction of the dimethyldichlorosilane.
Secondly, this disclosure sets up the analytic tower, and the material after the hydrolysis reaction flows into the membrane module of "people" style of calligraphy board combination after entering the analytic tower and makes the hydrogen chloride gas that produces in time escape, has prevented that the gas film from forming, is favorable to hydrolysis reaction forward going more to further improve the reaction yield of product.
Third, this disclosure sets up the circulating pump at hydrolysis reactor import, sets up the analysis tower at hydrolysis reactor export, and this combination setting can make dimethyldichlorosilane reaction more complete, effectively increases dimethyldichlorosilane's conversion rate, makes the acidity value greatly reduced of product moreover, and its acidity value is less than 1.2% (ordinary saturated acid hydrolysis product's acidity value is generally more than 3%).
The details of the resolving tower adopted in the present disclosure are shown in chinese patent with application number CN 201520127801.4.
One or more embodiments of this embodiment include a hydrogen chloride purification unit having an inlet coupled to the gas phase outlet of the stripper column.
In this series of examples, the liquid phase outlet of the hydrogen chloride purification unit is connected to the inlet of the separator. The separated hydrochloric acid and the partial hydrolysate carried away by the hydrogen chloride gas can be collected and reused.
In this series of embodiments, the hydrogen chloride purification apparatus includes a condenser.
In this series of embodiments, the hydrogen chloride purification apparatus includes a dryer.
In this series of embodiments, the hydrogen chloride purification apparatus includes a demister.
In the series of embodiments, the hydrogen chloride purification device comprises a condenser, a dryer and a demister which are sequentially connected according to the gas flow direction, wherein the inlet of the condenser is connected with the gas phase outlet of an analytical tower, the inlet of the dryer is connected with the gas phase outlet of the condenser, and the inlet of the demister is connected with the gas phase outlet of the dryer; the liquid phase outlet of the condenser, the liquid phase outlet of the dryer and the liquid phase outlet of the demister are all connected with the inlet of the separator.
In the series of embodiments, the system comprises a compressor pump, and an inlet of the compressor pump is connected with a gas phase outlet of the hydrogen chloride purification device. The hydrogen chloride gas is conveniently provided for users to use.
The hydrolysis reactor is similar in structure to a static mixer, and in order to increase the residence time of the material in the hydrolysis reactor, a filler is added in the hydrolysis reactor. In one or more embodiments of this embodiment, the hydrolysis reactor is a tubular structure, a plurality of mixing blades are installed in the tubular structure, and the tubular structure is filled with a filler.
In the series of embodiments, the two ends of the tubular structure are provided with the pattern plates, the pattern plates are perpendicular to the axis of the tubular structure, and the pattern plates are of plate-shaped structures provided with a plurality of through holes.
The other embodiment of the disclosure provides a process for hydrolyzing low-pressure dimethyldichlorosilane, and the system is provided, hydrochloric acid in a separator is pumped out by a circulating pump, the hydrochloric acid and dimethyldichlorosilane are premixed and then conveyed to a hydrolysis reactor for primary hydrolysis reaction, a material after the hydrolysis reaction enters an analytical tower, the material forms a liquid film in a film forming component of the analytical tower, hydrogen chloride in the liquid film is separated out and then subjected to secondary hydrolysis reaction, a liquid material after the reaction in the analytical tower enters the separator, the liquid material of the separator is divided into two layers, the lower layer is a water phase layer, the upper layer is an oil phase layer, the water phase layer is hydrochloric acid, the oil phase layer is a product, the reaction pressure is controlled to be below 50kPa, and the temperatures of the hydrolysis reactor and the analytical tower are controlled to be 30-50 ℃.
Through practical industrial verification, the process disclosed by the invention can not only reduce the reaction pressure, but also greatly improve the product yield, wherein the yield is higher than 99.9%, and simultaneously, the acidity value of the product can be greatly reduced, so that the acidity value of the first-stage reaction hydrolysate is below 1.2%.
In one or more embodiments of the present disclosure, water is added to the hydrochloric acid extracted from the separator to adjust the mass concentration of the hydrochloric acid to 33-35%.
In one or more embodiments of this embodiment, the hydrogen chloride gas evolved from the stripper column is subjected to condensation, drying, and/or dehazing. After the hydrogen chloride gas separated out from the desorption tower is sequentially subjected to condensation, drying and demisting treatment, the oil content of the hydrogen chloride gas can be reduced to be less than 5 ppm.
The hydrolysis product separated by the separator enters a subsequent purification washing system for purification.
The reaction pressures described in this disclosure are all gauge pressures. Gauge pressure refers to the number of total absolute pressures above ambient atmospheric pressure or the fraction of the pressure in the liquid that is above atmospheric pressure at some point.
In order to make the technical solutions of the present disclosure more clearly understood by those skilled in the art, the technical solutions of the present disclosure will be described in detail below with reference to specific examples and comparative examples.
Example 1
A system for hydrolyzing low-pressure dimethyldichlorosilane is shown in figure 1 and comprises a circulating pump 1, a hydrolysis reactor 2, a desorption tower 3, a condenser 4, a dryer 5, a demister 6, a separator 7 and a compressor pump 8.
The hydrolysis reactor 2 is of a tubular structure, a plurality of mixing blades are arranged in the tubular structure, and the tubular structure is filled with filler. The flower plates are arranged at two ends of the tubular structure and are perpendicular to the axis of the tubular structure, and the flower plates are of plate-shaped structures provided with a plurality of through holes.
Hydrochloric acid solution is used as a reaction carrier, is pressurized by a circulating pump 1, is mixed with dimethyldichlorosilane in a pipeline, then enters a hydrolysis reactor 2, is rapidly mixed in the hydrolysis reactor 2, and flows into a film forming component combined by a herringbone plate after the hydrolysis reactor 2 enters an analytical tower 3, so that reaction liquid is divided into a plurality of liquid films in the film forming component, and further completely reacts to separate out hydrogen chloride gas to produce a hydrolysate oil phase. The mixed solution of hydrolysate oil and hydrochloric acid enters a separator 7 from the bottom of the resolution tower 3, and the hydrolysate oil phase on the upper part of the separator 7 overflows and then enters a subsequent purification washing system; the lower hydrochloric acid is recycled after supplementing quantitative fresh water. The hydrogen chloride gas is discharged from the top of the desorption tower 3 and enters a condenser 4, the gas after partial acid water is condensed enters a dryer 5, the hydrogen chloride gas is freeze-dried and then passes through a demister 6, the amount of droplets with liquid in the hydrogen chloride gas entering a compressor pump 8 is controlled to be less than 5ppm, and the dried hydrogen chloride gas is pressurized and then conveyed to a user for use.
The specific process parameters are as follows:
the dimethyl feeding amount is 1 liter/hour, the hydrochloric acid circulating amount is 5 liters/hour, and the hydrochloric acid concentration is 35 percent. The pressure is controlled at about 50kPa during the test reaction, the reaction temperature is controlled at about 45 ℃, the oil phase of the reaction product stays in a separator for about 3 minutes, and the reaction product stands for 5 minutes after separation, and then the cycle ratio of hydrolysate is 54:46, and the acidity content in the hydrolysate is 0.3% (the saturated acid hydrolysis is generally more than 3%).
Example 2
The system of this example is the same as example 1.
The specific process parameters are as follows:
the dimethyl feeding amount is 1 liter/hour, the hydrochloric acid circulating amount is 3 liters/hour, and the hydrochloric acid concentration is 35 percent. The pressure is controlled at about 50KPa in the test reaction process, the reaction temperature is controlled at about 45 ℃, the oil phase of the reaction product stays in a separator for about 3 minutes, and stands for 5 minutes after separation, and the cycle ratio of hydrolysate is 51:49 and the acidity content in the hydrolysate is 0.5 percent (the saturated acid hydrolysis is generally more than 3 percent).
Example 3
The system of this example is the same as example 1.
The specific process parameters are as follows:
the dimethyl feeding amount is 1 liter/hour, the hydrochloric acid circulating amount is 5 liters/hour, and the hydrochloric acid concentration is 33 percent. The pressure is controlled at about 30KPa in the test reaction process, the reaction temperature is controlled at about 45 ℃, the oil phase of the reaction product stays in a separator for about 3 minutes, and stands for 5 minutes after separation, and the cycle ratio of the hydrolysate is 58:42 and the acidity content in the hydrolysate is 0.65 percent (the saturated acid hydrolysis is generally more than 3 percent).
Comparative example 1
The system of this comparative example is the same as the system of example 1, except that: the stripping column 3 is not provided.
The production was carried out according to the process parameters of example 1, with an acidity content of 3.2% in the hydrolysate.
Comparative example 2
The system of this comparative example is the same as the system of example 1, except that: the circulation pump 2 is not provided.
The production was carried out according to the process parameters of example 1, with an acidity content of 3.6% in the hydrolysate.
Comparative example 3
The system of this comparative example is the same as the system of example 1, except that: the analytical column 3 is not provided with a film formation module.
The production was carried out according to the process parameters of example 1, with an acidity content of 4.2% in the hydrolysate.
The above description is only a preferred embodiment of the present disclosure and is not intended to limit the present disclosure, and various modifications and changes may be made to the present disclosure by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present disclosure should be included in the protection scope of the present disclosure.
Claims (13)
1. A process for hydrolyzing low-pressure dimethyldichlorosilane is characterized in that the process is carried out in a system for hydrolyzing low-pressure dimethyldichlorosilane, the system comprises a hydrolysis reactor, a circulating pump, a desorption tower and a separator, an outlet of the hydrolysis reactor is connected with an inlet of the desorption tower, a liquid phase outlet of the desorption tower is connected with an inlet of the separator, a water phase outlet of the separator is connected with an inlet of the circulating pump, an outlet of the circulating pump is connected with an inlet of the hydrolysis reactor, a pipeline between the circulating pump and the hydrolysis reactor is connected with a conveying pipeline of dimethyldichlorosilane, a water replenishing pipeline is connected between the circulating pump and the separator,
the analysis tower comprises a distribution disc and a film forming component, the distribution disc is arranged at the middle-upper part in the falling film analysis tower, liquid distribution holes are formed in the distribution disc, the film forming component is arranged below the distribution disc and is formed by combining a plurality of groups of herringbone plates,
the separator is a vertically arranged cylindrical structure, the bottom of the separator is provided with a water phase outlet, the top of the separator is provided with an oil phase outlet,
the method comprises the following steps that hydrochloric acid in a separator is pumped out by a circulating pump and then premixed with dimethyl dichlorosilane, the mixture is conveyed to a hydrolysis reactor for primary hydrolysis reaction, a material after the hydrolysis reaction enters an analytical tower, the material forms a liquid film in a film forming component of the analytical tower, hydrogen chloride in the liquid film is separated out and then subjected to secondary hydrolysis reaction, a liquid material after reaction in the analytical tower enters the separator, the liquid material of the separator is divided into two layers, the lower layer is a water phase layer, the upper layer is an oil phase layer, the water phase layer is hydrochloric acid, the oil phase layer is a product, the reaction pressure is controlled to be below 50kPa, the pressure is gauge pressure, and the temperature of the hydrolysis reactor and the temperature of the analytical tower are controlled to be 30-50 ℃.
2. The process for the low pressure hydrolysis of dimethyldichlorosilane as claimed in claim 1 comprising a hydrogen chloride purification unit having an inlet connected to the gas phase outlet of the stripper column.
3. The process for the low pressure hydrolysis of dimethyldichlorosilane as claimed in claim 2 wherein the liquid phase outlet of the hydrogen chloride purification unit is connected to the inlet of the separator.
4. The process for the low pressure hydrolysis of dimethyldichlorosilane as claimed in claim 2 wherein the hydrogen chloride purification unit includes a condenser.
5. The process for the low pressure hydrolysis of dimethyldichlorosilane as claimed in claim 2 wherein the hydrogen chloride purification unit includes a dryer.
6. The process for the low pressure hydrolysis of dimethyldichlorosilane of claim 2 wherein the hydrogen chloride purification unit includes a mist eliminator.
7. The process of hydrolyzing low-pressure dimethyldichlorosilane according to claim 2 wherein the hydrogen chloride purification apparatus comprises a condenser, a dryer and a demister connected in sequence according to the gas flow direction, wherein the inlet of the condenser is connected with the gas phase outlet of the desorption tower, the inlet of the dryer is connected with the gas phase outlet of the condenser, the inlet of the demister is connected with the gas phase outlet of the dryer, and the liquid phase outlet of the condenser, the liquid phase outlet of the dryer and the liquid phase outlet of the demister are all connected with the inlet of the separator.
8. The process for the low pressure hydrolysis of dimethyldichlorosilane as claimed in claim 2 comprising a compressor pump, the inlet of said compressor pump being connected to the gas phase outlet of the hydrogen chloride purification unit.
9. The process for hydrolyzing low pressure dimethyldichlorosilane according to claim 2 wherein the hydrolysis reactor is a tubular structure, the tubular structure having a plurality of mixing blades mounted therein and filled with a filler.
10. The process for hydrolyzing low-pressure dimethyldichlorosilane according to claim 9, wherein the tubular structure is provided at both ends thereof with flower plates, the flower plates are perpendicular to the axis of the tubular structure, and the flower plates are plate-shaped structures provided with a plurality of through holes.
11. The process for hydrolyzing dimethyldichlorosilane according to claim 1, wherein the hydrochloric acid extracted from the separator is adjusted to 33 to 35% by weight by adding water.
12. The process for hydrolyzing dimethyldichlorosilane according to claim 1, wherein the hydrogen chloride gas separated out from the desorption tower is subjected to condensation, drying and/or demisting treatment.
13. The process for hydrolyzing low pressure dimethyldichlorosilane as claimed in claim 1, wherein the hydrogen chloride gas separated out from the desorption tower is sequentially subjected to condensation, drying and demisting treatment.
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| DE4343033A1 (en) * | 1993-12-16 | 1995-06-29 | Wacker Chemie Gmbh | Process for the preparation of polydimethylsiloxanes |
| CN100443488C (en) * | 2006-01-20 | 2008-12-17 | 中国石油天然气股份有限公司 | Method for reducing siloxane content in hydrolytic acid of dimethyl dichlorosilane |
| CN102153755A (en) * | 2008-12-08 | 2011-08-17 | 于淑芳 | Method for continuously producing hydrolysates by hydrolyzing methyl chlorosilane in concentrated acid |
| CN201704059U (en) * | 2010-05-14 | 2011-01-12 | 浙江恒业成有机硅有限公司 | Hydrogen chloride purifying device |
| CN102174200B (en) * | 2010-12-13 | 2012-11-14 | 山东东岳有机硅材料有限公司 | Method for hydrolyzing organochlorosilane |
| CN102210964B (en) * | 2011-06-17 | 2013-11-06 | 杭州中昊科技有限公司 | Gas phase silicon dioxide tail gas treatment process and system |
| CN103183827B (en) * | 2013-03-28 | 2015-08-19 | 青岛科技大学 | A kind of organochlorosilane continuous print Concentrated acid hydrolysis method |
| CN104163922B (en) * | 2014-07-21 | 2016-10-12 | 鲁西化工集团股份有限公司硅化工分公司 | A kind of dimethyldichlorosilane Concentrated acid hydrolysis technique under poised state |
| CN104277067B (en) * | 2014-09-18 | 2017-08-04 | 鲁西化工集团股份有限公司硅化工分公司 | Reduce the device and method of chloride ion content in Dimethyldichlorosilane hydrolysate |
| CN204638173U (en) * | 2015-03-05 | 2015-09-16 | 鲁西化工集团股份有限公司硅化工分公司 | A kind of dimethyldichlorosilane hydrolysis falling liquid film Analytic Tower |
| CN205933215U (en) * | 2016-06-23 | 2017-02-08 | 青海盐湖工业股份有限公司 | Hydrogen chloride drying device |
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