CN111004267A - Preparation method of hexamethyldisiloxane - Google Patents
Preparation method of hexamethyldisiloxane Download PDFInfo
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- CN111004267A CN111004267A CN201911282765.8A CN201911282765A CN111004267A CN 111004267 A CN111004267 A CN 111004267A CN 201911282765 A CN201911282765 A CN 201911282765A CN 111004267 A CN111004267 A CN 111004267A
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- hexamethyldisiloxane
- hydrochloric acid
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- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 title claims abstract description 157
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 317
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000007788 liquid Substances 0.000 claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 55
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 52
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 51
- 239000007789 gas Substances 0.000 claims abstract description 47
- 238000005406 washing Methods 0.000 claims abstract description 43
- 238000000926 separation method Methods 0.000 claims abstract description 38
- 239000005051 trimethylchlorosilane Substances 0.000 claims abstract description 35
- 239000000047 product Substances 0.000 claims abstract description 33
- 230000007062 hydrolysis Effects 0.000 claims abstract description 26
- 239000000413 hydrolysate Substances 0.000 claims abstract description 17
- 238000004064 recycling Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 108010009736 Protein Hydrolysates Proteins 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 65
- 238000003860 storage Methods 0.000 claims description 22
- 238000000746 purification Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 239000002585 base Substances 0.000 claims description 4
- 239000013589 supplement Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000460 chlorine Substances 0.000 abstract description 5
- 229910052801 chlorine Inorganic materials 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 description 13
- 239000011259 mixed solution Substances 0.000 description 12
- 239000000126 substance Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000012043 crude product Substances 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 5
- 238000010923 batch production Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000005046 Chlorosilane Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000011437 continuous method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- -1 polysiloxane Polymers 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 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
- C07F7/0838—Compounds with one or more Si-O-Si sequences
-
- 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
- C07F7/0838—Compounds with one or more Si-O-Si sequences
- C07F7/0872—Preparation and treatment thereof
- C07F7/0874—Reactions involving a bond of the Si-O-Si linkage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention provides a preparation method of hexamethyldisiloxane, A) concentrated hydrochloric acid and trimethylchlorosilane are sequentially conveyed into a hydrolysis reactor, and hydrolysis is carried out to obtain a hydrolysis product; the pressure of the hydrolysis reaction is 0.05-0.2 MPa; B) conveying the obtained hydrolysate to a heat exchanger for heating, then conveying the hydrolysate to a gas-liquid separation tower, separating hydrogen chloride gas from the hydrolysate, conveying the hydrogen chloride gas to a condenser, and collecting the hydrogen chloride gas from the top of the condenser; separating the upper oily liquid into a hexamethyldisiloxane water washing tank, and washing with water to obtain a crude hexamethyldisiloxane product; the lower hydrochloric acid water layer is conveyed to a hydrochloric acid intermediate tank for recycling; D) and conveying the obtained crude hexamethyldisiloxane product to a rectifying tower for separation to obtain hexamethyldisiloxane from the tower top. The invention does not produce low-concentration hydrochloric acid and improves the utilization rate of chlorine element.
Description
Technical Field
The invention belongs to the technical field of production of organic silicon chemicals, and particularly relates to a preparation method of hexamethyldisiloxane.
Background
With the rapid development of the organosilicon industry, the yield of the organosilicon chlorosilane monomer is increased more and more, and the total yield of domestic organosilicon monomer production enterprises at the end of the year is estimated to be about 2500 kt/a. Hexamethyldisiloxane is an important organosilicon primary raw material, and is often used as an end-capping agent for production of organosilicon silicone oil, production of polyether modified organosilicon oil, production of organosilicon release agent, or used as a cleaning agent for silicon rubber, medicines, gas chromatography stationary liquid, analytical reagents, water repellent, medical electronic elements and the like. The Si-O-Si bond in the hexamethyldisiloxane molecular chain structure has higher chemical bond energy (460.5kJ/mol), and the polysiloxane prepared by using the hexamethyldisiloxane molecular chain structure as the end sealing agent has better thermal stability and chemical stability.
CN103319519B discloses a method for producing hexamethyldisiloxane by using organosilicon azeotrope, comprising: (1) distilling the organic silicon azeotrope to obtain an intermediate mixture; (2) carrying out batch esterification reaction on the intermediate mixture, heating and distilling the reaction liquid, and collecting fractions with boiling points lower than 80 ℃ to obtain a crude product of trimethylchlorosilane; (3) hydrolyzing the crude trimethylchlorosilane product, and separating from the hydrolysate to obtain hexamethyldisiloxane. The method has the advantages of low price of raw materials, sufficient supply of goods, mild conditions in the reaction process, stable process and high continuous production efficiency. However, the method produces more hydrochloric acid through hydrolysis, the concentration of the hydrochloric acid is low, the recovery and the use are limited, the waste of chlorine elements is caused, and the energy consumption of low-level hydrogen chloride recovery is very large.
Disclosure of Invention
The invention aims to provide a preparation method of hexamethyldisiloxane, which does not generate low-concentration hydrochloric acid, improves the utilization rate of chlorine element, and reduces the unit consumption of trimethylchlorosilane.
The invention provides a preparation method of hexamethyldisiloxane, which comprises the following steps:
A) sequentially conveying concentrated hydrochloric acid and trimethylchlorosilane into a hydrolysis reactor for hydrolysis reaction to obtain a hydrolysate;
the pressure of the hydrolysis reaction is 0-0.2 MPa;
B) conveying the obtained hydrolysate to a heat exchanger for heating, then entering a gas-liquid separation tower, separating hydrogen chloride gas from the hydrolysate, entering a purification condenser, collecting the hydrogen chloride gas from the top of the purification condenser, and obtaining a mixture of hydrochloric acid and hexamethyldisiloxane from the bottom of the purification condenser;
the bottom of the gas-liquid separation tower obtains a mixture of hexamethyldisiloxane and concentrated hydrochloric acid;
C) conveying a mixture of hexamethyldisiloxane and concentrated hydrochloric acid obtained from the bottom of the gas-liquid separation tower and a mixture of hydrochloric acid and hexamethyldisiloxane obtained from the bottom of the condenser to a delayer for layering; separating the upper oily liquid into a hexamethyldisiloxane water washing tank, washing with water to obtain a crude hexamethyldisiloxane product, and feeding the crude hexamethyldisiloxane product into a hexamethyldisiloxane intermediate tank;
the lower hydrochloric acid water layer is conveyed to a hydrochloric acid intermediate tank for recycling;
D) and conveying the obtained crude hexamethyldisiloxane product to a rectifying tower for separation, obtaining gas-phase hexamethyldisiloxane from the tower top, and condensing to obtain hexamethyldisiloxane.
Preferably, the temperature of the hydrolysis reaction is 5-30 ℃.
Preferably, the temperature of the hydrolysate subjected to heat exchange in the step B) is 30-80 ℃.
Preferably, the pressure in the gas-liquid separation column is normal pressure.
Preferably, the crude hexamethyldisiloxane in the step D) is firstly conveyed to a drying tower for drying and dewatering, and then conveyed to a rectifying tower for separation.
Preferably, the acid water obtained by washing in step C) is directly fed to a hydrochloric acid intermediate tank, and is mixed with the lower hydrochloric acid water separated by the laminator in step C) in the hydrochloric acid intermediate tank, and fed to the hydrolysis reactor to supplement water required for the hydrolysis reaction.
Preferably, the washing liquid used for washing in the step C) is water or a weak base aqueous solution;
the weak base is one or more of sodium carbonate, sodium bicarbonate and potassium carbonate.
Preferably, the mass concentration of the concentrated hydrochloric acid is more than 10%.
Preferably, the mass ratio of the hydrochloric acid to the trimethylchlorosilane is 1: (0.7-4).
Preferably, a preparation apparatus is used comprising:
the hydrolysis reactor is provided with a trimethylchlorosilane inlet, a hydrochloric acid inlet and a product outlet, and the trimethylchlorosilane is communicated with a trimethylchlorosilane storage tank; the hydrochloric acid inlet is communicated with a hydrochloric acid storage tank; the product outlet is communicated with the heat exchanger;
the discharge hole of the heat exchanger is communicated with the inlet of the gas-liquid separator;
the gas-liquid separator is provided with a top outlet and a bottom outlet, and the top outlet is used for discharging hydrochloric acid gas and communicated with the purification condenser; the bottom outlet is used for discharging a mixture of concentrated hydrochloric acid and hexamethyldisiloxane and is communicated with the delayer 7;
the top outlet of the purification condenser is communicated with a hydrogen chloride gas storage tank; the bottom outlet of the purification condenser is communicated with the delayer;
the delaminating device is provided with an upper-layer liquid outlet and a lower-layer liquid outlet, the upper-layer liquid outlet is communicated with the hexamethyldisiloxane intermediate tank, and the lower-layer liquid outlet is communicated with the hydrochloric acid storage tank;
the hexamethyldisiloxane intermediate tank is provided with a bottom outlet communicated with the hydrochloric acid storage tank, and a middle outlet is communicated with the drying tower 9, the rectifying tower 10, the hexamethyldisiloxane condenser 11 and the hexamethyldisiloxane storage tank in sequence.
The invention provides a preparation method of hexamethyldisiloxane, which comprises the following steps: A) sequentially conveying concentrated hydrochloric acid and trimethylchlorosilane into a hydrolysis reactor for hydrolysis reaction to obtain a hydrolysate; the pressure of the hydrolysis reaction is 0.05-0.2 MPa; B) conveying the obtained hydrolysate to a heat exchanger for heating, then entering a gas-liquid separation tower, separating hydrogen chloride gas from the hydrolysate, entering a condenser, collecting the hydrogen chloride gas from the top of the condenser, and obtaining a mixture of hydrochloric acid and hexamethyldisiloxane from the bottom of the condenser; the bottom of the gas-liquid separation tower obtains a mixture of hexamethyldisiloxane and concentrated hydrochloric acid; C) conveying a mixture of hexamethyldisiloxane and concentrated hydrochloric acid obtained from the bottom of the gas-liquid separation tower and a mixture of hydrochloric acid and MM obtained from the bottom of the condenser to a delayer for layering; separating the upper oily liquid into a hexamethyldisiloxane water washing tank, washing with water to obtain a crude hexamethyldisiloxane product, and feeding the crude hexamethyldisiloxane product into a hexamethyldisiloxane intermediate tank; the lower hydrochloric acid water layer is conveyed to a hydrochloric acid intermediate tank for recycling; D) and conveying the obtained crude hexamethyldisiloxane product to a rectifying tower for separation, obtaining gas-phase hexamethyldisiloxane from the tower top, and condensing to obtain hexamethyldisiloxane. The invention hydrolyzes under the pressure condition, the generated hydrogen chloride is dissolved in water, and the hydrogen chloride is released out to automatically become hydrogen chloride gas after the pressure is changed into normal pressure. The method produces the hydrogen chloride gas by-product while preparing the hexamethyldisiloxane, does not produce low-concentration hydrochloric acid, solves the problem of recycling hydrochloric acid produced in the hydrolysis process, improves the utilization rate of chlorine element, and reduces the unit consumption of the trimethylchlorosilane.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a preparation apparatus used in the present invention,
wherein, 1, a trimethyl chlorosilane storage tank; 2. a hydrolysis reactor; 3. a heat exchanger; 4. a gas-liquid separator; 5. purifying the condenser; 6. a hydrogen chloride gas storage tank; 7. a delayer; 8. a hexamethyldisiloxane intermediate tank; 9. a drying tower; 10. a rectifying tower; 11. a hexamethyldisiloxane condenser; 12. a hexamethyldisiloxane storage tank; 13. a hexamethyldisiloxane rectification feed pump; 14. a hexamethyldisiloxane crude product conveying pump; 15. a mixed liquid delivery pump; 16. a hydrochloric acid delivery pump; 17. a hydrochloric acid storage tank; 18. a hydrochloric acid feed pump; 19. a trimethylchlorosilane transfer pump.
Detailed Description
The invention provides a preparation method of hexamethyldisiloxane, which comprises the following steps:
A) sequentially conveying concentrated hydrochloric acid and trimethylchlorosilane into a hydrolysis reactor for hydrolysis reaction to obtain a hydrolysate;
the pressure of the hydrolysis reaction is 0.05-0.2 MPa;
B) conveying the obtained hydrolysate to a heat exchanger for heating, then entering a gas-liquid separation tower, separating hydrogen chloride gas from the hydrolysate, entering a condenser, collecting the hydrogen chloride gas from the top of the condenser, and obtaining a mixture of hydrochloric acid and hexamethyldisiloxane from the bottom of the condenser;
the bottom of the gas-liquid separation tower obtains a mixture of hexamethyldisiloxane and concentrated hydrochloric acid;
C) conveying a mixture of hexamethyldisiloxane and concentrated hydrochloric acid obtained from the bottom of the gas-liquid separation tower and a mixture of hydrochloric acid and MM obtained from the bottom of the condenser to a delayer for layering; separating the upper oily liquid into a hexamethyldisiloxane water washing tank, washing with water to obtain a crude hexamethyldisiloxane product, and feeding the crude hexamethyldisiloxane product into a hexamethyldisiloxane intermediate tank;
the lower hydrochloric acid water layer is conveyed to a hydrochloric acid intermediate tank for recycling;
D) and conveying the obtained crude hexamethyldisiloxane product to a rectifying tower for separation, obtaining gas-phase hexamethyldisiloxane from the tower top, and condensing to obtain hexamethyldisiloxane.
In the present invention, hexamethyldisiloxane is prepared using the apparatus of figure 1, which comprises a hydrolysis reactor 2 provided with a trimethylchlorosilane inlet in communication with a trimethylchlorosilane storage tank via a trimethylchlorosilane transfer pump 19.
The hydrolysis reactor 2 is also provided with a hydrochloric acid inlet which is communicated with a hydrochloric acid storage tank through a hydrochloric acid feeding pump 18;
the hydrolysis reactor 2 is also provided with a product outlet which is communicated with the heat exchanger 3 through a pipeline;
the discharge hole of the heat exchanger 3 is communicated with the inlet of the gas-liquid separator 4, the gas-liquid separator 4 is also provided with a top outlet and a bottom outlet, the top outlet is used for discharging hydrochloric acid gas, and the bottom outlet is used for discharging a mixture of concentrated hydrochloric acid and hexamethyldisiloxane;
the top outlet of the gas-liquid separator is communicated with a purification condenser 5, and the top outlet of the purification condenser is communicated with a hydrogen chloride gas storage tank 6; the bottom outlet of the purification condenser is communicated with a delaminating device 7 and is used for conveying the mixture of hydrochloric acid and hexamethyldisiloxane at the bottom into the delaminating device 7.
The bottom outlet of the gas-liquid separator is communicated with the delaminating device 7 and is used for conveying the mixture of the hexamethyldisiloxane at the bottom and the concentrated hydrochloric acid into the delaminating device 7.
The delaminating device 7 is provided with an upper-layer liquid outlet and a lower-layer liquid outlet, the upper-layer liquid outlet is communicated with the hexamethyldisiloxane intermediate tank 8, and the lower-layer liquid outlet is communicated with the hydrochloric acid storage tank 17.
The hexamethyldisiloxane intermediate tank 8 is provided with a bottom outlet communicated with the hydrochloric acid storage tank, and a middle outlet communicated with the drying tower 9, the rectifying tower 10, the hexamethyldisiloxane condenser 11 and the hexamethyldisiloxane storage tank in sequence.
In the invention, the hydrolysis reactor is a Venturi mixer, a static mixer, a common tubular reactor, or a common pot type reactor with stirring, or other equipment capable of bearing pressure and mixing materials. In particular, the mixer can withstand pressures of-0.1 MPa to 0.3 MPa.
The rectifying tower is preferably a packed or trayed rectifying tower.
The hexamethyldisiloxane is preferably prepared according to the following steps;
1) conveying concentrated hydrochloric acid into a hydrolysis reactor by a pump, conveying trimethylchlorosilane into the hydrolysis reactor in which the concentrated hydrochloric acid exists by the pump, mixing the trimethylchlorosilane with the concentrated hydrochloric acid, contacting water, and hydrolyzing to generate hexamethyldisiloxane and hydrogen chloride gas;
2) the mixed material of hexamethyldisiloxane, hydrogen chloride gas and concentrated hydrochloric acid obtained in the step 1 enters a heat exchanger for heating, and then enters a gas-liquid separation tower from the tower bottom; hydrogen chloride gas is separated from the mixture, overflows from the top of the separation tower and enters a condenser; collecting hydrogen chloride gas from the top of the condenser, and recovering a mixture of entrained hydrochloric acid and hexamethyldisiloxane from the bottom of the condenser to enter a delayer through condensation.
3) 2, obtaining a mixture of hexamethyldisiloxane and concentrated hydrochloric acid at the bottom of the gas-liquid separation tower, conveying the mixture into a delaminator through a pump, standing and layering to form an oil-water layer; separating the lower hydrochloric acid water layer, conveying to a hydrochloric acid intermediate tank, and recycling; and separating the upper oily liquid layer, introducing the upper oily liquid layer into a hexamethyldisiloxane water washing tank, washing the hexamethyldisiloxane water washing tank with water or alkali liquor until the hexamethyldisiloxane water washing tank is neutral to obtain a crude hexamethyldisiloxane product, and introducing the crude hexamethyldisiloxane product into a hexamethyldisiloxane intermediate tank.
4) And (3) conveying the crude hexamethyldisiloxane product obtained in the step (3) to a drying tower through a pump for drying and dewatering, conveying the crude hexamethyldisiloxane product to a rectifying tower through a pump for separation, obtaining gas-phase hexamethyldisiloxane from the top of the tower, and condensing to obtain a product hexamethyldisiloxane.
5) And (3) conveying the lower-layer hydrochloric acid subjected to standing and layering in the step 3 to a hydrochloric acid intermediate tank through a pump for recycling.
6) And 3, directly conveying acid water obtained by washing hexamethyldisiloxane in the water washing tank to a hydrochloric acid intermediate tank through a pump, mixing the acid water with hydrochloric acid obtained by separation in the gas-liquid separation tank in the step 5, conveying the mixed acid water to the mixed hydrolyzer in the step 1 through the pump, and supplementing water required by the hydrolysis reaction in the step 1.
In the invention, the temperature of the hydrolysis reaction is preferably 5-30 ℃, more preferably 10-25 ℃, and most preferably 15-20 ℃; the pressure of the hydrolysis reaction is preferably 0.05 to 0.2MPa, and more preferably 0.1 to 0.15 MPa.
In the present invention, the concentrated hydrochloric acid is saturated hydrochloric acid under the system pressure condition, or hydrochloric acid with a hydrochloric acid concentration of more than 10%, specifically, in an embodiment of the present invention, the mass concentration of the concentrated hydrochloric acid may be 30%.
In the present invention, the mass ratio of the concentrated hydrochloric acid to the trimethylchlorosilane is preferably ×.
In the invention, the temperature of the hydrolysate after heat exchange by the heat exchanger is preferably 30-80 ℃, more preferably 40-60 ℃, and most preferably 50 ℃. And heating the hydrolysate to enter a gas-liquid separation tower, wherein the system pressure is atmospheric pressure, separating hydrogen chloride gas in the mixture from the system, and condensing and separating the entrained hydrochloric acid and hexamethyldisiloxane by a condenser to obtain pure hydrogen chloride gas. The hydrogen chloride gas obtained by the invention can be used as other industrial raw materials.
In the present invention, the washing liquid used for the washing is preferably water or a weak alkali aqueous solution; the weak base is one or more of sodium carbonate, sodium bicarbonate and potassium carbonate.
In the present invention, the rectification is preferably a common rectification method such as vacuum rectification, atmospheric rectification or pressure rectification.
In the present invention, the hexamethyldisiloxane can be prepared by a continuous method or a batch-wise method.
The hexamethyldisiloxane prepared by the invention can be used for preparing hydrogen-containing telomeric oil or methyl silicone oil which is an intermediate of modified silicone oil.
The invention provides a preparation method of hexamethyldisiloxane, which comprises the following steps: A) sequentially conveying concentrated hydrochloric acid and trimethylchlorosilane into a hydrolysis reactor for hydrolysis reaction to obtain a hydrolysate; the pressure of the hydrolysis reaction is 0.05-0.2 MPa; B) conveying the obtained hydrolysate to a heat exchanger for heating, then entering a gas-liquid separation tower, separating hydrogen chloride gas from the hydrolysate, entering a condenser, collecting the hydrogen chloride gas from the top of the condenser, and obtaining a mixture of hydrochloric acid and hexamethyldisiloxane from the bottom of the condenser; the bottom of the gas-liquid separation tower obtains a mixture of hexamethyldisiloxane and concentrated hydrochloric acid; C) conveying a mixture of hexamethyldisiloxane and concentrated hydrochloric acid obtained from the bottom of the gas-liquid separation tower and a mixture of hydrochloric acid and MM obtained from the bottom of the condenser to a delayer for layering; separating the upper oily liquid into a hexamethyldisiloxane water washing tank, washing with water to obtain a crude hexamethyldisiloxane product, and feeding the crude hexamethyldisiloxane product into a hexamethyldisiloxane intermediate tank; the lower hydrochloric acid water layer is conveyed to a hydrochloric acid intermediate tank for recycling; D) and conveying the obtained crude hexamethyldisiloxane product to a rectifying tower for separation, obtaining gas-phase hexamethyldisiloxane from the tower top, and condensing to obtain hexamethyldisiloxane. The invention hydrolyzes under the pressure condition, the generated hydrogen chloride is dissolved in water, and the hydrogen chloride is released out to automatically become hydrogen chloride gas after the pressure is changed into normal pressure. The method produces the hydrogen chloride gas by-product while preparing the hexamethyldisiloxane, does not produce low-concentration hydrochloric acid, solves the problem of recycling hydrochloric acid produced in the hydrolysis process, improves the utilization rate of chlorine element, and reduces the unit consumption of the trimethylchlorosilane.
In order to further illustrate the present invention, the following examples are provided to describe the preparation method of hexamethyldisiloxane provided by the present invention, but should not be construed as limiting the scope of the present invention.
Example 1 a continuous process produces hexamethyldisiloxane.
1) 108 parts of trimethylchlorosilane with the content of 99 percent are continuously conveyed into a mixer hydrolyzer with 36.5 percent of concentrated hydrochloric acid and the pressure of 0.1MPa by a shield pump, and the trimethylchlorosilane and the water in the hydrochloric acid are subjected to hydrolysis reaction to obtain a mixture of hexamethyldisiloxane, the concentrated hydrochloric acid and hydrogen chloride gas generated by hydrolysis.
2) The mixed material enters a heat exchanger through self pressure, is heated to 50 ℃, enters a gas-liquid separation tower, is separated from the mixture by 37 parts of hydrogen chloride gas, enters a condenser, is condensed and purified, and is collected to obtain 35 parts of hydrogen chloride gas.
3) And (3) obtaining a mixture of 121 parts of hexamethyldisiloxane and concentrated hydrochloric acid at the bottom of the gas-liquid separation tower, mixing the mixture with 2 parts of the recovery liquid obtained in the step (6) in a layering tank to obtain 123 parts of the mixture, standing the mixture for layering, feeding 82.5 parts of the upper-layer liquid into a water washing tank, washing the upper-layer liquid with 9 parts of water to be neutral to obtain 82 parts of crude hexamethyldisiloxane and 9.5 parts of washing water.
4) 82 parts of crude hexamethyldisiloxane passes through a preheater, the outlet temperature is 105 ℃, and the hexamethyldisiloxane is pumped into a rectifying tower to be separated under normal pressure to obtain 80 parts of product hexamethyldisiloxane and 2 parts of high-boiling-point substances.
5) The mixture of hexamethyldisiloxane and concentrated hydrochloric acid is kept in a layering tank for layering, 40.5 parts of lower concentrated hydrochloric acid is mixed with 9.5 parts of washing water obtained from a washing tank, and then the mixture is conveyed to a hydrochloric acid intermediate tank by a pump to obtain 50 parts of hydrochloric acid, and the hydrochloric acid is conveyed to a mixer hydrolyzer by the pump for recycling.
The parts described in this example are mass flow per unit time by weight.
In this example, 80 parts of hexamethyldisiloxane was obtained, 35 parts of hydrogen chloride gas was obtained, and no fresh diluted hydrochloric acid was produced.
Example 2 a batch process produces hexamethyldisiloxane.
1) 108 parts of trimethylchlorosilane with the content of 99 percent is continuously conveyed into a mixer containing 50 parts of 36.5 percent concentrated hydrochloric acid by a shielding pump to perform hydrolysis reaction with water in the hydrochloric acid to obtain 158 parts of a mixture of hexamethyldisiloxane, the concentrated hydrochloric acid and hydrogen chloride gas generated by hydrolysis, and the pressure of the mixer is continuously increased to finally reach 0.12MPa.
2) And after the trimethyl chlorosilane is fed, closing the feeding valve and stopping the conveying pump. The mixed material enters a heat exchanger through self pressure to be heated to 50 ℃, then enters a gas-liquid separation tower, 37 parts of hydrogen chloride gas is separated from the mixture and is absorbed, enters a condenser from the tower top, and is condensed and purified to obtain 35 parts of hydrogen chloride gas.
3) And (4) condensing the hydrogen chloride gas, collecting to obtain 2 parts of mixed solution of hydrochloric acid and hexamethyldisiloxane, adding the mixed solution into a delayer, mixing the mixed solution with the mixture obtained in the step (4), and standing for layering.
4) And (3) separating the tower bottom to obtain a mixture of 121 parts of hexamethyldisiloxane and concentrated hydrochloric acid, mixing the mixture with the mixed solution obtained in the step (3) in a delayer to obtain 123 parts of mixture, standing and delaminating, allowing 82.5 parts of upper-layer liquid to enter a washing tank, washing with 9 parts of water and then delaminating, allowing 82 parts of neutral hexamethyldisiloxane crude product to be obtained in the upper layer and 9.5 parts of washing water to be obtained in the lower layer, conveying the mixture to a hydrochloric acid intermediate tank through a pump, and allowing the mixture to enter a mixer for later use.
5) And (4) standing the mixture of hexamethyldisiloxane and concentrated hydrochloric acid obtained in the step (4) for layering to obtain 40.5 parts of lower-layer concentrated hydrochloric acid, and mixing the lower-layer concentrated hydrochloric acid with the washing water obtained in the step (4) to obtain 50 parts of hydrochloric acid. The next batch is conveyed to the mixer through the pump for recycling.
6) And (4) heating the crude hexamethyldisiloxane 82 obtained in the step (4) to 105 ℃ by a preheater, and then separating the crude hexamethyldisiloxane in a rectifying tower under reduced pressure to obtain 80 parts of hexamethyldisiloxane as a product and 2 parts of high-boiling-point substances.
The parts described in this example are mass by weight.
This example yielded 35 parts of hydrogen chloride gas along with 80 parts of hexamethyldisiloxane. 50 parts of hydrochloric acid with the concentration of 30.5 percent can be recycled in the next batch of production to supplement water required by the hydrolysis reaction.
Example 3 a batch process produces hexamethyldisiloxane.
1) 108 parts of trimethylchlorosilane with the content of 99 percent is continuously conveyed into a mixer containing 70 parts of 20.4 percent concentrated hydrochloric acid by a shielding pump to perform hydrolysis reaction with water in the hydrochloric acid to obtain 178 parts of a mixture of hexamethyldisiloxane, the concentrated hydrochloric acid and hydrogen chloride gas generated by hydrolysis, and the pressure of the mixer is continuously increased to finally reach 0.08MPa.
2) And after the trimethyl chlorosilane is fed, closing the feeding valve and stopping the conveying pump. The mixed material enters a heat exchanger through self pressure to be heated to 80 ℃, then enters a gas-liquid separation tower, 30 parts of hydrogen chloride gas are separated and absorbed from the mixture, enters a condenser from the tower top, and is condensed and purified to obtain 29 parts of hydrogen chloride gas.
3) And (4) condensing the hydrogen chloride gas, collecting 1 part of mixed solution of hydrochloric acid and hexamethyldisiloxane, feeding the mixed solution into a delayer, mixing the mixed solution with the mixture obtained in the step (4), and standing for layering.
4) And (3) separating the tower bottom to obtain a mixture of 148 parts of hexamethyldisiloxane and concentrated hydrochloric acid, mixing the mixture with the mixed solution obtained in the step (3) in a delayer for 149 parts, standing for layering, allowing 82.5 parts of upper-layer liquid to enter a washing tank, washing with 12 parts of water, layering, allowing 82 parts of neutral hexamethyldisiloxane crude product to be obtained in the upper layer and 12.5 parts of washing water to be obtained in the lower layer, conveying the mixture to a hydrochloric acid intermediate tank through a pump, and allowing the mixture to enter a mixer for later use in the next batch.
5) And (3) standing the mixture of hexamethyldisiloxane and concentrated hydrochloric acid obtained in the step (4) for layering to obtain 66.5 parts of lower-layer concentrated hydrochloric acid, and mixing the lower-layer concentrated hydrochloric acid with the water washing water obtained in the step (4) to obtain 79 parts of hydrochloric acid. The next batch is conveyed to the mixer through the pump for recycling.
6) And (4) heating the crude hexamethyldisiloxane 82 obtained in the step (4) to 105 ℃ by a preheater, and then separating the crude hexamethyldisiloxane in a rectifying tower under reduced pressure to obtain 80 parts of hexamethyldisiloxane as a product and 2 parts of high-boiling-point substances.
The parts described in this example are mass by weight.
This example yielded 29 parts of hydrogen chloride gas along with 80 parts of hexamethyldisiloxane. 79 portions of hydrochloric acid with the concentration of 27.5 percent can be recycled in the next production, and the water required by the hydrolysis reaction is supplemented.
Example 4 a batch process produces hexamethyldisiloxane.
1) 108 parts of trimethylchlorosilane with the content of 99 percent is continuously conveyed into a mixer containing 80 parts of 10 percent concentrated hydrochloric acid by a shield pump to perform hydrolysis reaction with water in the hydrochloric acid to obtain 188 parts of a mixture of hexamethyldisiloxane, the concentrated hydrochloric acid and hydrogen chloride gas generated by hydrolysis, and the pressure of the mixer is continuously increased to finally reach 0.08MPa.
2) And after the trimethyl chlorosilane is fed, closing the feeding valve and stopping the conveying pump. The mixed material enters a heat exchanger through self pressure to be heated to 70 ℃, then enters a gas-liquid separation tower, 15 parts of hydrogen chloride gas are separated and absorbed from the mixture, enters a condenser from the tower top, and is condensed and purified to obtain 14 parts of hydrogen chloride gas.
3) And (4) condensing the hydrogen chloride gas, collecting 1 part of mixed solution of hydrochloric acid and hexamethyldisiloxane, feeding the mixed solution into a delayer, mixing the mixed solution with the mixture obtained in the step (4), and standing for layering.
4) And (3) separating the tower bottom to obtain 173 parts of a mixture of hexamethyldisiloxane and concentrated hydrochloric acid, mixing the mixture with the mixed solution in the step (3) in a delaminating device to obtain 174 parts, standing and delaminating, allowing 82.5 parts of upper-layer liquid to enter a washing tank, washing with 6 parts of water and then delaminating, allowing 82 parts of neutral hexamethyldisiloxane crude product to be obtained in the upper layer and 6.5 parts of washing water to be obtained in the lower layer, conveying the mixture to a hydrochloric acid intermediate tank through a pump, and allowing the mixture to enter a mixer for later use in the.
5) And (3) standing the mixture of hexamethyldisiloxane and concentrated hydrochloric acid obtained in the step (4) for layering to obtain 91.5 parts of lower-layer concentrated hydrochloric acid, and mixing the lower-layer concentrated hydrochloric acid with the washing water obtained in the step (4) to obtain 98 parts of hydrochloric acid. The next batch is conveyed to the mixer through the pump for recycling.
6) And (4) heating the crude hexamethyldisiloxane 82 obtained in the step (4) to 105 ℃ by a preheater, and then separating the crude hexamethyldisiloxane in a rectifying tower under reduced pressure to obtain 80 parts of hexamethyldisiloxane as a product and 2 parts of high-boiling-point substances.
The parts described in this example are mass by weight.
In this example, 80 parts of hexamethyldisiloxane and 14 parts of hydrogen chloride gas were obtained. 98 portions of hydrochloric acid with the concentration of 31 percent can be recycled in the next batch of production to supplement water required by the hydrolysis reaction.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of hexamethyldisiloxane comprises the following steps:
A) sequentially conveying concentrated hydrochloric acid and trimethylchlorosilane into a hydrolysis reactor for hydrolysis reaction to obtain a hydrolysate;
the pressure of the hydrolysis reaction is 0-0.2 MPa;
B) conveying the obtained hydrolysate to a heat exchanger for heating, then entering a gas-liquid separation tower, separating hydrogen chloride gas from the hydrolysate, entering a purification condenser, collecting the hydrogen chloride gas from the top of the purification condenser, and obtaining a mixture of hydrochloric acid and hexamethyldisiloxane from the bottom of the purification condenser;
the bottom of the gas-liquid separation tower obtains a mixture of hexamethyldisiloxane and concentrated hydrochloric acid;
C) conveying a mixture of hexamethyldisiloxane and concentrated hydrochloric acid obtained from the bottom of the gas-liquid separation tower and a mixture of hydrochloric acid and hexamethyldisiloxane obtained from the bottom of the condenser to a delayer for layering; separating the upper oily liquid into a hexamethyldisiloxane water washing tank, washing with water to obtain a crude hexamethyldisiloxane product, and feeding the crude hexamethyldisiloxane product into a hexamethyldisiloxane intermediate tank;
the lower hydrochloric acid water layer is conveyed to a hydrochloric acid intermediate tank for recycling;
D) and conveying the obtained crude hexamethyldisiloxane product to a rectifying tower for separation, obtaining gas-phase hexamethyldisiloxane from the tower top, and condensing to obtain hexamethyldisiloxane.
2. The method according to claim 1, wherein the temperature of the hydrolysis reaction is 5 to 30 ℃.
3. The preparation method of claim 1, wherein the temperature of the hydrolysate subjected to heat exchange in the step B) is 30-80 ℃.
4. The production method according to claim 1, wherein the pressure in the gas-liquid separation column is atmospheric pressure.
5. The preparation method according to claim 1, wherein the crude hexamethyldisiloxane in the step D) is conveyed to a drying tower for drying and dewatering, and then conveyed to a rectifying tower for separation.
6. The method according to claim 1, wherein the acid water obtained by washing in step C) is directly fed to a hydrochloric acid intermediate tank, and the acid water is mixed with the lower hydrochloric acid water separated from the separator in step C) in the hydrochloric acid intermediate tank and fed to the hydrolysis reactor to supplement water required for the hydrolysis reaction.
7. The process according to claim 1, wherein the washing liquid used for the washing in step C) is water or a weak alkali aqueous solution;
the weak base is one or more of sodium carbonate, sodium bicarbonate and potassium carbonate.
8. The method according to claim 1, wherein the concentrated hydrochloric acid is present at a concentration of > 10% by mass.
9. The preparation method according to claim 8, wherein the mass ratio of the hydrochloric acid to the trimethylchlorosilane is 1: (0.7-4).
10. The production method according to claim 1, characterized in that a production apparatus comprising:
the hydrolysis reactor is provided with a trimethylchlorosilane inlet, a hydrochloric acid inlet and a product outlet, and the trimethylchlorosilane is communicated with a trimethylchlorosilane storage tank; the hydrochloric acid inlet is communicated with a hydrochloric acid storage tank; the product outlet is communicated with the heat exchanger;
the discharge hole of the heat exchanger is communicated with the inlet of the gas-liquid separator;
the gas-liquid separator is provided with a top outlet and a bottom outlet, and the top outlet is used for discharging hydrochloric acid gas and communicated with the purification condenser; the bottom outlet is used for discharging a mixture of concentrated hydrochloric acid and hexamethyldisiloxane and is communicated with the delayer 7;
the top outlet of the purification condenser is communicated with a hydrogen chloride gas storage tank; the bottom outlet of the purification condenser is communicated with the delayer;
the delaminating device is provided with an upper-layer liquid outlet and a lower-layer liquid outlet, the upper-layer liquid outlet is communicated with the hexamethyldisiloxane intermediate tank, and the lower-layer liquid outlet is communicated with the hydrochloric acid storage tank;
the hexamethyldisiloxane intermediate tank is provided with a bottom outlet communicated with the hydrochloric acid storage tank, and a middle outlet is communicated with the drying tower 9, the rectifying tower 10, the hexamethyldisiloxane condenser 11 and the hexamethyldisiloxane storage tank in sequence.
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| CN114213660A (en) * | 2021-12-30 | 2022-03-22 | 杭州崇耀科技发展有限公司 | Preparation method and catalyst of organic silicon oil |
| CN114478610A (en) * | 2022-01-25 | 2022-05-13 | 杭州四马化工科技有限公司 | Production process of vinyl silane |
| CN114751930A (en) * | 2022-05-17 | 2022-07-15 | 山东博苑医药化学股份有限公司 | Method for recovering hexamethyldisiloxane from waste solvent containing trimethylsilylether and hexamethyldisiloxane |
| CN115193146A (en) * | 2022-07-14 | 2022-10-18 | 内蒙古恒业成有机硅有限公司 | Oil-water layering tank for hydrolysis of dimethyldichlorosilane |
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