CN113996256A - Method and device for treating dimethyl dichlorosilane hydrolysate - Google Patents
Method and device for treating dimethyl dichlorosilane hydrolysate Download PDFInfo
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- CN113996256A CN113996256A CN202111341697.5A CN202111341697A CN113996256A CN 113996256 A CN113996256 A CN 113996256A CN 202111341697 A CN202111341697 A CN 202111341697A CN 113996256 A CN113996256 A CN 113996256A
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- 239000000413 hydrolysate Substances 0.000 title claims abstract description 81
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 108
- 239000000203 mixture Substances 0.000 claims abstract description 102
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 97
- 239000000126 substance Substances 0.000 claims abstract description 76
- 238000009835 boiling Methods 0.000 claims abstract description 54
- 239000005046 Chlorosilane Substances 0.000 claims abstract description 23
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 16
- 108010009736 Protein Hydrolysates Proteins 0.000 claims abstract description 12
- 239000004094 surface-active agent Substances 0.000 claims description 15
- 238000005191 phase separation Methods 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract description 45
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract description 45
- 230000000694 effects Effects 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 9
- 239000012071 phase Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 12
- 238000005406 washing Methods 0.000 description 11
- 239000000460 chlorine Substances 0.000 description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- XKJMJYZFAWYREL-UHFFFAOYSA-N hexadecamethylcyclooctasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XKJMJYZFAWYREL-UHFFFAOYSA-N 0.000 description 4
- 230000001965 increasing effect Effects 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 description 2
- IUMSDRXLFWAGNT-UHFFFAOYSA-N Dodecamethylcyclohexasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 IUMSDRXLFWAGNT-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229940050176 methyl chloride Drugs 0.000 description 2
- 238000007142 ring opening reaction Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- VEYJKODKHGEDMC-UHFFFAOYSA-N dichloro(trichlorosilyl)silicon Chemical compound Cl[Si](Cl)[Si](Cl)(Cl)Cl VEYJKODKHGEDMC-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- HTDJPCNNEPUOOQ-UHFFFAOYSA-N hexamethylcyclotrisiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O1 HTDJPCNNEPUOOQ-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00004—Scale aspects
- B01J2219/00006—Large-scale industrial plants
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Gas Separation By Absorption (AREA)
Abstract
The invention discloses a method and a device for treating a dimethyl dichlorosilane hydrolysate, wherein the method comprises the following steps: performing hydrolysis reaction on dimethyl dichlorosilane and concentrated hydrochloric acid to obtain a hydrolysate; separating the hydrolysate to obtain a first mixture, wherein the first mixture comprises aqueous hydrogen chloride; and absorbing water in the first mixture by using a high-boiling-point substance, wherein the high-boiling-point substance contains chlorosilane. In the method for treating the hydrolysate of dimethyldichlorosilane, which is provided by the embodiment of the invention, the hydrolysate of dimethyldichlorosilane and concentrated hydrochloric acid is separated to obtain a first mixture, the first mixture comprises aqueous hydrogen chloride, water in the first mixture can be absorbed by a high-boiling-point substance, chlorosilane is contained in the high-boiling-point substance, and the high-boiling-point substance is difficult to volatilize due to high boiling point and can be rapidly hydrolyzed when encountering water, so that water in the hydrogen chloride can be removed, the water removal efficiency is high, the water removal effect is good, and no new impurities are introduced.
Description
Technical Field
The invention belongs to the technical field of organic silicon, and particularly relates to a method and a device for treating a dimethyl dichlorosilane hydrolysate.
Background
In the organic silicon production, in the hydrolysis process of the dimethyldichlorosilane, HCl gas discharged from the top of the tower contains a small amount of water, HCl needs to be dehydrated after being recovered and then participates in the synthesis of methyl chloride again, and due to the existence of water, the subsequent utilization is affected, the existing water removal effect is poor, and the cost is high.
Disclosure of Invention
The embodiment of the invention aims to provide a method and a device for treating a dimethyl dichlorosilane hydrolysate, which are used for solving the problem that water contained in HCl gas discharged from the top of a tower in a dimethyl dichlorosilane hydrolysis process is not easy to remove and can influence subsequent utilization.
In a first aspect, an embodiment of the present invention provides a method for treating a dimethyldichlorosilane hydrolysate, including:
performing hydrolysis reaction on dimethyl dichlorosilane and concentrated hydrochloric acid to obtain a hydrolysate;
separating the hydrolysate to obtain a first mixture, wherein the first mixture comprises aqueous hydrogen chloride;
and absorbing water in the first mixture by using a high-boiling-point substance, wherein the high-boiling-point substance contains chlorosilane.
Wherein the high boiling substance comprises chlorosilane having two silicon atoms and/or two or more silicon atoms.
Wherein the temperature of the high-boiling-point substance is 10-35 ℃.
Wherein, still include:
and separating the hydrolysate to obtain a second mixture, wherein the second mixture is the hydrolysate containing water.
Wherein, still include:
the second mixture is phase separated and an aqueous surfactant is added during the phase separation to obtain a hydrolysate.
Wherein the step of absorbing water in the first mixture with a high boiling substance comprises:
demisting the first mixture by a demister;
and absorbing the water in the demisted first mixture by using the high-boiling residues.
Wherein, after the step of absorbing the water in the first mixture by using the high boiling substance, the method further comprises the following steps:
the first mixture after absorbing water with the high boiling substance is compressed by a compressor.
In a second aspect, an embodiment of the present invention provides an apparatus for processing a dimethyldichlorosilane hydrolysate, including:
the hydrolysis reactor is used for carrying out hydrolysis reaction on the dimethyl dichlorosilane and the concentrated hydrochloric acid;
the separation device is used for separating the hydrolysate to obtain a first mixture, and the first mixture comprises aqueous hydrogen chloride;
and the absorption device is used for absorbing the water in the first mixture by utilizing a high-boiling-point substance, and the high-boiling-point substance contains chlorosilane.
Wherein, the device still includes:
and the phase separator is used for separating the hydrolysate to obtain a second mixture, and the second mixture is the hydrolysate containing water.
Wherein, the device still includes:
the demisting device is used for demisting the first mixture;
and the absorption device is used for absorbing the water in the demisted first mixture by using the high-boiling-point substance.
Wherein, the device still includes:
and the compression device is used for compressing the first mixture after the water is absorbed by the high-boiling-point substance.
The method for treating the dimethyl dichlorosilane hydrolysate comprises the following steps: performing hydrolysis reaction on dimethyl dichlorosilane and concentrated hydrochloric acid to obtain a hydrolysate; separating the hydrolysate to obtain a first mixture, wherein the first mixture comprises aqueous hydrogen chloride; and absorbing water in the first mixture by using a high-boiling-point substance, wherein the high-boiling-point substance contains chlorosilane. In the method for treating the hydrolysate of dimethyldichlorosilane, which is provided by the embodiment of the invention, the hydrolysate of dimethyldichlorosilane and concentrated hydrochloric acid is separated to obtain a first mixture, the first mixture comprises aqueous hydrogen chloride, water in the first mixture can be absorbed by a high-boiling-point substance, chlorosilane is contained in the high-boiling-point substance, and the high-boiling-point substance is difficult to volatilize due to high boiling point and can be rapidly hydrolyzed when encountering water, so that water in the hydrogen chloride can be removed, the water removal efficiency is high, the water removal effect is good, and no new impurities are introduced.
Drawings
FIG. 1 is a schematic diagram of a connection of a processing apparatus according to an embodiment of the present invention.
Reference numerals
A hydrolysis reactor 10;
a separation device 20;
an absorbing device 30;
a phase separator 40;
a defogging device 50;
a compression device 60.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The terms first, second and the like in the description and in the claims of the present invention are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that embodiments of the invention may be practiced otherwise than as specifically illustrated and described herein. In addition, "and/or" in the specification and claims means at least one of connected objects, a character "/" generally means that a preceding and succeeding related objects are in an "or" relationship.
The method for treating the dimethyl dichlorosilane hydrolysate comprises the following steps:
performing hydrolysis reaction on dimethyl dichlorosilane and concentrated hydrochloric acid to obtain a hydrolysate;
separating the hydrolysate to obtain a first mixture, wherein the first mixture comprises aqueous hydrogen chloride;
and absorbing water in the first mixture by using a high-boiling-point substance, wherein the high-boiling-point substance contains chlorosilane.
In the method for treating the hydrolysate of dimethyldichlorosilane, which is provided by the embodiment of the invention, the hydrolysate of dimethyldichlorosilane and concentrated hydrochloric acid is separated to obtain a first mixture, the first mixture comprises aqueous hydrogen chloride, water in the first mixture can be absorbed by a high-boiling-point substance, chlorosilane is contained in the high-boiling-point substance, and the high-boiling-point substance is difficult to volatilize due to high boiling point and can be rapidly hydrolyzed when encountering water, so that water in the hydrogen chloride can be removed, the water removal efficiency is high, the water removal effect is good, and no new impurities are introduced.
The water in the first mixture can be removed by a washing tower, high-boiling-point substances can pass through the top of the washing tower, the temperature of the high-boiling-point substances can be 25 ℃, the first mixture can be introduced from the top of the washing tower, the first mixture contains a large amount of hydrogen chloride gas and a small amount of water, and the hydrogen chloride flows to the top of the washing tower, so that the first mixture is in contact with the high-boiling-point substances, and the high-boiling-point substances can absorb the water in the hydrogen chloride. In the first mixture, a small amount of D3 (hexamethylcyclotrisiloxane) is still contained, D3 accumulates in the whole production system, and when the accumulation is high, the pipeline in the system is easy to be blocked, and D3 can be removed while water is removed because D3 in hydrogen chloride can be absorbed by high boiling substances. The chlorosilane in the high-boiling residue is hydrolyzed quickly when encountering water, more hydroxyl groups are arranged in the hydrolyzed high-boiling residue, and the hydroxyl groups in the high-boiling residue can react, so that the viscosity of the high-boiling residue is increased, the effect of absorbing D3 in the first mixture can be enhanced, water in hydrogen chloride can be removed, the water removal efficiency is high, and the water removal effect is good. Before absorption, the water content in HCl is about 1000ppm, the D3 content is about 0.4% -0.8%, after water in hydrogen chloride is absorbed by high-boiling substances, the water content in the hydrogen chloride can be reduced to below 10ppm, the D3 can be reduced to below 100ppm, and the water and D3 removing effect is good. In addition, a small amount of decamethylcyclopentasiloxane (D5), dodecamethylcyclohexasiloxane (D6), decatetramethylcyclohexasiloxane (D7), and hexadecamethylcyclooctasiloxane (D8) may be entrained in the first mixture, and a small amount of decamethylcyclopentasiloxane (D5), dodecamethylcyclohexasiloxane (D6), decatetramethylcyclohexasiloxane (D7), and hexadecamethylcyclooctasiloxane (D8) may be removed by adsorption of a high boiling substance.
Water in the hydrogen chloride is removed through the high-boiling-point substances, the high-boiling-point substances contain chlorosilane, and the chlorine in the chlorosilane can be hydrolyzed when meeting water, so that the water is removed. Chlorine atoms in the chlorosilane are changed into hydroxyl groups, macromolecular polymers can be generated when the hydroxyl groups are condensed, the polymers can absorb D3 in the hydrogen chloride, and high-boiling residues can also absorb D3 in the hydrogen chloride. The dried hydrogen chloride can be compressed by a compressor and then can be used in the synthesis of methyl chloride. The organics were similarly compatible and high boilers could remove D3. The water is removed through the high-boiling-point substance, the generated polymer can be beneficial to increasing the molecular weight, the polymer can absorb D3, and the polymer is not easy to enter hydrogen chloride in the high-boiling-point substance.
In some embodiments, the high boiling substance may include a chlorosilane having two silicon atoms and/or more than two silicon atoms. For example, the chlorosilane can include one or more of hexamethylhexachlorodisilane, tetramethyloctachlorodisilane, and heptamethyl pentachlorodisilane.
In some embodiments, the high boiling substance may include (CH)3)3SiCH2SiCl2Me、MeCl2SiCH2SiCl2Me、Cl3SiSiCl3、Me2ClSiSiCl3、MeCl2SiOSiCl2Me、Me2ClSiCH2SiClMe2、PhSiCl3、MeCH2CH2SiCl3、MeCH2CH2MeSiCl2、Me2ClSiCH2SiCl3、Cl3SiCH2SiCl3Me represents a methyl group and Ph represents a phenyl group. The mass percentage of chlorosilane in the high-boiling residue can be greater than or equal to 80 percent so as to better remove water and adsorb D3.
In some embodiments, the temperature of the high boiling substance may be 10 to 35 ℃, for example, 25 ℃, and water and D3 in the hydrogen chloride may be absorbed by the high boiling substance at normal temperature without heating, thereby reducing energy consumption and cost, and the lower temperature does not volatilize components in the high boiling substance. The boiling point of the high boiling substance may be 80 ℃ or higher, alternatively, the boiling point of the high boiling substance may be 120 ℃ or higher, enhancing the effect of removing water and adsorbing D3. The high boiling substance may include (CH)3)3SiCH2SiCl2Me、MeCl2SiCH2SiCl2Me、Cl3SiSiCl3、Me2ClSiSiCl3、MeCl2SiOSiCl2Me、Me2ClSiCH2SiClMe2、PhSiCl3、MeCH2CH2SiCl3、MeCH2CH2MeSiCl2、Me2ClSiCH2SiCl3And Cl3SiCH2SiCl3。
In some embodiments, before the high boiling substance is used, the high boiling substance may be distilled at 80 ℃ for 30-50 minutes, and then the temperature of the high boiling substance is reduced to 10-35 ℃ so as to volatilize and remove some low boiling point components and avoid impurities in the hydrogen chloride.
In one embodiment, the high boiling substance Comprises (CH)3)3SiCH2SiCl2Me、MeCl2SiCH2SiCl2Me、Cl3SiSiCl3、Me2ClSiSiCl3、MeCl2SiOSiCl2Me、Me2ClSiCH2SiClMe2、PhSiCl3、MeCH2CH2SiCl3、MeCH2CH2MeSiCl2、Me2ClSiCH2SiCl3And Cl3SiCH2SiCl3Before the high-boiling-point substance is used, the high-boiling-point substance is distilled at 80 ℃ for 40 minutes, and then the temperature of the high-boiling-point substance is reduced to 25 ℃ so as to volatilize and remove some low-boiling-point components. The water content in HCl before absorption is 984ppm, the D3 content is about 0.536%, after the water in the hydrogen chloride is absorbed by high-boiling-point substances, the water content in the hydrogen chloride can be reduced to 8ppm, the D3 can be reduced to 86ppm, and the removal effect of the water and the D3 is better.
In an embodiment of the invention, the method further comprises:
and separating the hydrolysate to obtain a second mixture, wherein the second mixture is the hydrolysate containing water.
In some embodiments, the method further comprises:
the second mixture is phase separated and an aqueous surfactant is added during the phase separation to obtain a hydrolysate. The second mixture comprises hydrolysate of oil phase, and the hydrolysate comprises ring hydrolysate and linear hydrolysate.
The hydrolysate can be separated by a separation tower, the ring hydrolysate and the linear hydrolysate in the tower bottom components contain a small amount of water and HCl, the hydrolysate is introduced into a phase separator to separate the hydrolysate from a water phase, and the ring hydrolysate is easy to open during the separation process due to the fact that the separation time needs a certain time, so that the loop ratio is reduced. In the separation process, the water-based surfactant is added, and the surfactant is hydrophilic, so that an isolation film can be formed between the hydrolysate (oil phase) and the water phase, the contact of the hydrolysate and the water phase is reduced, the ring opening of a ring body is reduced, and the ring-line ratio is improved. The surfactant is dissolved in water, is easy to remove in the subsequent water washing process, and has no influence on hydrolysate.
When the second mixture is subjected to phase separation, the second mixture comprises a ring body hydrolysate, a line body hydrolysate and an aqueous phase (hydrochloric acid), wherein the hydrolysate accounts for 70-80%, and the hydrochloric acid accounts for 20-30%. In the phase separation process, before the surfactant is added for separation, the ratio of the ring body hydrolysate to the line body hydrolysate in the hydrolysate is 3: 7; the phase separation time is 20-60 min, the temperature is normal temperature, the surfactant can be N-dimethyl N-octylamine, and the addition amount of the surfactant is 0.1-0.5% of the total amount of hydrolysate. After the addition of the surfactant, the ratio of the ring body hydrolysate to the linear body hydrolysate can be increased to 5:5 to 7:3 after the phase separation of the hydrolysates.
In some embodiments, the step of absorbing water in the first mixture with a high boiling point substance comprises:
demisting the first mixture by a demister;
the water in the demisted first mixture is absorbed by the high-boiling-point substances, the mist foam of the first mixture is removed by the demister, and the subsequent water in the demisted first mixture is absorbed by the high-boiling-point substances.
In an embodiment of the present invention, after the step of absorbing water in the first mixture with a high boiling substance, the method further comprises:
the first mixture obtained after the water is absorbed by the high-boiling-point substances is compressed by the compressor, impurities in the first mixture can be removed by compressing the first mixture by the compressor, and the impurities in the hydrogen chloride are further removed.
During the application process, the hydrolysate can be separated to obtain a second mixture, and the second mixture comprises water containing hydrogen chloride and hydrolysate;
in some embodiments, the method further comprises: the second mixture is phase separated and an aqueous surfactant is added during the phase separation to obtain a hydrolysate.
The hydrolysate obtained after phase separation may be subjected to water removal to remove water containing hydrogen chloride. That is, the hydrolysate obtained after phase separation contains a small amount of hydrochloric acid and needs to be removed. The hydrolysate containing aqueous hydrogen chloride solution may be subjected to cryogenic cooling to-10 ℃ to-40 ℃ to crystallize the aqueous hydrogen chloride solution in the hydrolysate, and the hydrolysate containing crystals may be filtered to remove the crystals. The solidification crystallization can appear in aqueous hydrogen chloride solution under the lower temperature, and the aqueous hydrogen chloride solution dispersion after the solidification crystallization can detach the crystallization in the hydrolysate through filtering for aqueous hydrogen chloride solution separates away from the hydrolysate, and the aqueous hydrogen chloride solution in the hydrolysate can effectively be got rid of to above-mentioned scheme, removes water and hydrogen chloride, avoids water and hydrogen chloride to cause the influence to subsequent technology, and the crystallization of isolating can be retrieved and become aqueous hydrogen chloride solution and utilize again.
Before the step of cryogenically cooling the hydrolysate containing the aqueous hydrogen chloride solution to-10 ℃ to-40 ℃ to crystallize the aqueous hydrogen chloride solution in the hydrolysate, the method may further comprise: deionized water was added to the hydrolysate containing aqueous hydrogen chloride solution to adjust the content of hydrogen chloride in the aqueous hydrogen chloride solution to 0.5 to 5%. Can adjust the content of hydrogen chloride in the hydrogen chloride aqueous solution to 0.5-5% through adding deionized water to the hydrolysate that contains the hydrogen chloride aqueous solution for the concentration of hydrogen chloride in the hydrogen chloride aqueous solution reduces, does not need lower temperature just can make the hydrogen chloride aqueous solution crystallization solidify, can reduce the energy consumption, reduce cost.
As shown in fig. 1, an embodiment of the present invention provides an apparatus for processing a dimethyldichlorosilane hydrolysate, including: the hydrolysis reactor 10 can be used for hydrolysis reaction of dimethyl dichlorosilane and concentrated hydrochloric acid; separation apparatus 20 may be used to separate the hydrolysate to obtain a first mixture comprising aqueous hydrogen chloride; the absorption device 30 can be used to absorb water in the first mixture by using a high boiling substance having chlorosilane therein.
Dimethyldichlorosilane and concentrated hydrochloric acid can hydrolyze in hydrolysis reactor 10, and separator 20 can separate the hydrolysate, obtains first mixture, first mixture includes hydrous hydrogen chloride, can utilize high boiling thing to absorb water in the first mixture in absorbing device 30, have chlorosilane in the high boiling thing, because high boiling thing's boiling point is higher, be difficult to volatilize, hydrolysis takes place when chlorosilane in the high boiling thing meets water fast, can remove the water in the hydrogen chloride, and it is efficient to remove water, and it is effectual to remove water, can not introduce new impurity.
The absorption device 30 may include a washing tower, water in the first mixture may be removed by the washing tower, a high boiling substance may pass through the top of the washing tower, the temperature of the high boiling substance may be 25 ℃, the first mixture may be introduced from the top of the washing tower, the first mixture contains a large amount of hydrogen chloride gas and a small amount of water, and hydrogen chloride flows to the top of the washing tower, so that the first mixture contacts with the high boiling substance, and the high boiling substance may absorb water in the hydrogen chloride. D3 in hydrogen chloride can be absorbed by the high boiling substance, and D3 can be removed while removing water. The chlorosilane in the high-boiling residue is hydrolyzed quickly when encountering water, more hydroxyl groups are arranged in the hydrolyzed high-boiling residue, and the hydroxyl groups in the high-boiling residue can react, so that the viscosity of the high-boiling residue is increased, the effect of absorbing D3 in the first mixture can be enhanced, water in hydrogen chloride can be removed, the water removal efficiency is high, and the water removal effect is good.
In some embodiments, the apparatus further comprises: a phase separator 40 for separating the hydrolysate to obtain a second mixture, wherein the second mixture is the hydrolysate containing water.
When the second mixture is subjected to phase separation, an aqueous surfactant is added during the phase separation to obtain a hydrolysate. The second mixture comprises hydrolysate of oil phase, and the hydrolysate comprises ring hydrolysate and linear hydrolysate. And (3) introducing the second mixture into a phase separator to separate the hydrolysate and the water phase, and adding an aqueous surfactant during the separation process, wherein the surfactant is hydrophilic, so that an isolation membrane can be formed between the hydrolysate (oil phase) and the water phase, the contact between the hydrolysate and the water phase is reduced, the ring opening of a ring body is reduced, and the ring-to-line ratio is improved. The surfactant is dissolved in water, is easy to remove in the subsequent water washing process, and has no influence on hydrolysate.
Optionally, the apparatus further comprises: the demisting device 50, the demisting device 50 can be used for demisting the first mixture, and the absorption device can be used for absorbing the water in the demisted first mixture by using the high-boiling-point substance.
Optionally, the apparatus further comprises: the compressing device 60, the compressing device 60 can be used for compressing the first mixture after absorbing water by the high boiling point substance. The first mixture obtained after the water is absorbed by the high-boiling-point substances is compressed by the compressor, impurities in the first mixture can be removed by compressing the first mixture by the compressor, and the impurities in the hydrogen chloride are further removed.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (11)
1. A method for treating a dimethyl dichlorosilane hydrolysate, which is characterized by comprising the following steps:
performing hydrolysis reaction on dimethyl dichlorosilane and concentrated hydrochloric acid to obtain a hydrolysate;
separating the hydrolysate to obtain a first mixture, wherein the first mixture comprises aqueous hydrogen chloride;
and absorbing water in the first mixture by using a high-boiling-point substance, wherein the high-boiling-point substance contains chlorosilane.
2. The process according to claim 1, wherein the high boilers comprise chlorosilanes having two silicon atoms and/or more than two silicon atoms.
3. The process according to claim 1, wherein the temperature of the high boilers is from 10 to 35 ℃.
4. The method of claim 1, further comprising:
and separating the hydrolysate to obtain a second mixture, wherein the second mixture is the hydrolysate containing water.
5. The method of claim 4, further comprising:
the second mixture is phase separated and an aqueous surfactant is added during the phase separation to obtain a hydrolysate.
6. The method of claim 4, wherein the step of absorbing water in the first mixture with a high boiling point substance comprises:
demisting the first mixture by a demister;
and absorbing the water in the demisted first mixture by using the high-boiling residues.
7. The method of claim 4, further comprising, after the step of absorbing water in the first mixture with a high boiling substance:
the first mixture after absorbing water with the high boiling substance is compressed by a compressor.
8. An apparatus for treating a dimethyldichlorosilane hydrolysate, comprising:
the hydrolysis reactor is used for carrying out hydrolysis reaction on the dimethyl dichlorosilane and the concentrated hydrochloric acid;
the separation device is used for separating the hydrolysate to obtain a first mixture, and the first mixture comprises aqueous hydrogen chloride;
and the absorption device is used for absorbing the water in the first mixture by utilizing a high-boiling-point substance, and the high-boiling-point substance contains chlorosilane.
9. The apparatus of claim 8, further comprising:
and the phase separator is used for separating the hydrolysate to obtain a second mixture, and the second mixture is the hydrolysate containing water.
10. The apparatus of claim 8, further comprising:
the demisting device is used for demisting the first mixture;
and the absorption device is used for absorbing the water in the demisted first mixture by using the high-boiling-point substance.
11. The apparatus of claim 8, further comprising:
and the compression device is used for compressing the first mixture after the water is absorbed by the high-boiling-point substance.
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