CN117534697B - Preparation process and preparation system of tri-tert-butoxy silanol - Google Patents
Preparation process and preparation system of tri-tert-butoxy silanol Download PDFInfo
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- CN117534697B CN117534697B CN202410027054.0A CN202410027054A CN117534697B CN 117534697 B CN117534697 B CN 117534697B CN 202410027054 A CN202410027054 A CN 202410027054A CN 117534697 B CN117534697 B CN 117534697B
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- tank body
- tert
- butoxysilanol
- grinding
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- HLDBBQREZCVBMA-UHFFFAOYSA-N hydroxy-tris[(2-methylpropan-2-yl)oxy]silane Chemical compound CC(C)(C)O[Si](O)(OC(C)(C)C)OC(C)(C)C HLDBBQREZCVBMA-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title abstract description 27
- PCLIMKBDDGJMGD-UHFFFAOYSA-N N-bromosuccinimide Chemical compound BrN1C(=O)CCC1=O PCLIMKBDDGJMGD-UHFFFAOYSA-N 0.000 claims abstract description 91
- 238000003756 stirring Methods 0.000 claims abstract description 82
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000005052 trichlorosilane Substances 0.000 claims abstract description 47
- 239000000463 material Substances 0.000 claims abstract description 42
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 35
- MFRIHAYPQRLWNB-UHFFFAOYSA-N sodium tert-butoxide Chemical compound [Na+].CC(C)(C)[O-] MFRIHAYPQRLWNB-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 238000005192 partition Methods 0.000 claims abstract description 25
- 238000010992 reflux Methods 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 238000003860 storage Methods 0.000 claims abstract description 18
- 230000000903 blocking effect Effects 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims description 65
- 238000006243 chemical reaction Methods 0.000 claims description 55
- 238000000034 method Methods 0.000 claims description 28
- 230000008569 process Effects 0.000 claims description 26
- 238000007789 sealing Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 16
- 238000000926 separation method Methods 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 238000001514 detection method Methods 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 11
- 239000011261 inert gas Substances 0.000 claims description 11
- 239000012074 organic phase Substances 0.000 claims description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
- 230000005540 biological transmission Effects 0.000 claims description 9
- 239000012043 crude product Substances 0.000 claims description 9
- 238000005481 NMR spectroscopy Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- 238000005292 vacuum distillation Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 238000010586 diagram Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 230000005311 nuclear magnetism Effects 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000003961 organosilicon compounds Chemical class 0.000 description 2
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 2
- 238000000427 thin-film deposition Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- VQPFDLRNOCQMSN-UHFFFAOYSA-N bromosilane Chemical compound Br[SiH3] VQPFDLRNOCQMSN-UHFFFAOYSA-N 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
-
- 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 System
- C07F7/02—Silicon compounds
- C07F7/04—Esters of silicic acids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8361—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating
- B01F33/83613—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating by grinding or milling
-
- 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
- B01J19/18—Stationary reactors having moving elements inside
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention discloses a preparation process and a preparation system of tri-tert-butoxy silanol, which relate to the technical field of tri-tert-butoxy silanol preparation and comprise the following steps: s1, adding n-hexane solvent and sodium tert-butoxide into a tank body, and putting the tank body into a normal pressure reflux device to stir by a stirring shaft arranged in the tank body; s2, controlling the heating temperature of the tank body to be a T1 value, adding trichlorosilane into a cavity separated by a partition plate in the tank body, adding N-bromosuccinimide raw material into a first storage cavity in the tank body, wherein a material leakage hole is formed in the partition plate, and driving a blocking structure to block the material leakage Kong Jiaoti when a stirring shaft is used for stirring, so that the trichlorosilane liquid raw material quantitatively drops and is dropwise added through the material leakage hole.
Description
Technical Field
The invention relates to the technical field of preparation of tri-tert-butoxy silanol, in particular to a preparation process and a preparation system of tri-tert-butoxy silanol.
Background
Tri-t-butoxysilanol is an organosilicon compound and has wide application in the vapor deposition field. The tri-t-butoxysilanol may be used as a precursor material in a PECVD process for depositing silicon oxide (SiOx) films, and in particular, the tri-t-butoxysilanol may be reacted with oxygen in a PECVD reaction chamber to form SiOx films. The method can prepare a high-quality, uniform and compact SiOx film, and the film can be used for preparing semiconductor devices such as an insulating layer, an isolating layer, a dielectric layer and the like, has excellent electrical property and optical property, and therefore, has wide application in the fields of microelectronics, optoelectronics, solar cells and the like.
Chemical vapor deposition is the most widely applied thin film deposition technology in the fields of integrated circuits and semiconductors, and as the semiconductor industry is rapidly developed, the scale is continuously enlarged, the technology is continuously improved, the requirements on equipment related to thin film deposition are rapidly increased, the market demand of organosilicon compounds is also in an increasing trend, and the current synthesis process has a plurality of process steps and low synthesis efficiency, so that the requirements of the market cannot be met.
Disclosure of Invention
The invention aims to provide a preparation process and a preparation system of tri-tert-butoxy silanol, which solve the defects in the prior art.
In order to achieve the above object, the present invention provides the following technical solutions: a process for preparing tri-t-butoxysilanol comprising:
s1, adding n-hexane solvent and sodium tert-butoxide into a tank body, and putting the tank body into a normal pressure reflux device to stir by a stirring shaft arranged in the tank body;
s2, controlling the heating temperature of the tank body to be a T1 value, adding trichlorosilane into a cavity separated by a partition plate in the tank body, adding N-bromosuccinimide raw material into a first storage cavity in the tank body, wherein a material leakage hole is formed in the partition plate, and driving a blocking structure to block the material leakage Kong Jiaoti when a stirring shaft is used for stirring, so that the trichlorosilane liquid raw material quantitatively drops and is dropwise added through the material leakage hole, and heating to T2 and keeping reflux for 8 hours after the dropwise adding is finished;
s3, when the stirring shaft drives the plugging structure to control leakage Kong Dijia trichlorosilane, the stirring shaft synchronously drives the grinding part to grind the N-bromosuccinimide raw material, the grinded N-bromosuccinimide powder enters a cavity separated by a partition plate in the tank body, enters the tank body through a leakage hole, the temperature is controlled to be T3, the stirring reaction is carried out for 6 hours, after the stirring is finished, sodium carbonate and distilled water are added, the temperature is controlled to be T4, and the stirring reaction is carried out for 8 hours;
s4, separating the mixed solution obtained in the step S3 to obtain an organic phase, adding anhydrous sodium sulfate, drying, filtering to obtain a filtrate, removing solvent n-hexane under normal pressure and then reducing pressure, and finally evaporating the crude product of the tri-tert-butoxysilanol under absolute pressure;
and S5, purifying the obtained crude tri-tert-butoxysilanol by vacuum distillation, and removing front and rear fractions according to the proportion of 3-6% of the content of the obtained crude tri-tert-butoxysilanol to obtain a middle fraction which is the finished tri-tert-butoxysilanol product.
Preferably, all of the above S1 to S5 are performed under an inert gas atmosphere, and the n-hexane in the above S1 may be used after drying and water removal.
Preferably, in the above S2, the temperature range of T1 is-10 to 0 ℃, the temperature of T2 is 70 to 75 ℃, and the equivalent ratio of trichlorosilane to sodium tert-butoxide in the above S2 is 1:1.05 to 1.3 times.
Preferably, in the above step S3, the temperature of T3 is in the range of 60to 70 ℃ and the temperature of T4 is 80 ℃.
Preferably, the three-tert-butoxysilanol end product obtained in S5 is subjected to nuclear magnetic resonance and ICP detection by washing with water three times and drying with anhydrous sodium sulfate.
The preparation system for the tri-tert-butoxy silanol realizes the preparation process of the tri-tert-butoxy silanol, and comprises a tank body, wherein a stirring shaft is arranged in the tank body, and the preparation system further comprises:
a polishing section;
the central tube is movably inserted into the tank body, and after solid raw materials are added into the grinding part, the central tube receives the transmission of the stirring shaft so as to drive the grinding part to crush the raw materials through the central tube;
the separation plate is arranged in the tank body, a plurality of material leakage holes are uniformly formed in the separation plate, and liquid raw materials are contained above the separation plate;
the blocking structure is arranged on the central tube, and is corresponding to different rotation speeds of the stirring shaft, the blocking structure is provided with a first state and a second state, the blocking structure alternately blocks the upper end and the lower end of the material leakage hole in the first state, liquid raw materials quantitatively fall through the material leakage hole, the grinding part is passively opened in the second state, and solid raw materials in the grinding part fall through the material leakage hole.
Preferably, the grinding part comprises a first grinding body, a second grinding body and a movable door, wherein the first grinding body is fixedly arranged on the upper part of the inner wall of the tank body, a first storage cavity is formed in the upper part of the first grinding body, the second grinding body is fixedly arranged outside the central pipe, a second storage cavity is formed in the lower parts of the first grinding body and the second grinding body, the movable door is arranged on the lower part of the first grinding body, the movable door is used for plugging the second storage cavity in a first state, and the movable door is opened in a second state.
Preferably, the upper portion of division board is provided with the funnel, the central upper portion of division board is provided with protruding platform, the position setting of weeping hole is between funnel and protruding platform.
Preferably, the plugging structure comprises a first connecting arm, a first tension member, a second connecting arm, a first plugging strip, a rotary sleeve and a second plugging strip, wherein the first connecting arm is connected to the central tube in a sliding mode, the second connecting arm is connected to the first connecting arm in a sliding mode, the first tension member applies a tension force to the second connecting arm towards the central tube, the first plugging strip is fixedly connected with a swing arm, the upper end of the swing arm is connected to the second connecting arm, the rotary sleeve is connected to the lower portion of the partition plate in a rotating mode, the rotary sleeve is connected with the central tube through a transmission portion, and the second plugging strip is fixedly installed outside the rotary sleeve.
Preferably, a wedge is fixedly installed at one end of the second connecting arm, in the first state, the wedge is abutted against the lower part of the movable door, and in the second state, the contact point between the wedge and the movable door moves downwards.
In the technical scheme, the preparation process and the preparation system of the tri-tert-butoxy silanol provided by the invention have the advantages of simple process, fewer reaction steps, reasonable raw material proportion and fewer generated wastes, so that the cost of the preparation raw materials is reduced, the equipment investment cost and the subsequent preparation cost can be effectively reduced in the industrialized promotion, and the production concept of energy conservation and environmental protection is met.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings may be obtained according to these drawings for a person having ordinary skill in the art.
FIG. 1 is a schematic diagram showing the overall structure of a process and a system for preparing tri-t-butoxysilanol according to the present invention;
FIG. 2 is a cross-sectional view of a tank of a process and system for preparing tri-t-butoxysilanol according to the present invention;
FIG. 3 is a cross-sectional view of a divider plate of a process and system for preparing tri-t-butoxysilanol according to the present invention;
FIG. 4 is a schematic diagram of a plugging mechanism of a process and a system for preparing tri-t-butoxysilanol according to the present invention;
FIG. 5 is an enlarged schematic view of the process and system for preparing tri-t-butoxysilanol of the present invention at A in FIG. 4;
FIG. 6 is a schematic diagram showing the structure of a process and a system for preparing tri-t-butoxysilanol according to the present invention in a first state;
FIG. 7 is an enlarged schematic view of the process and system for preparing tri-t-butoxysilanol of the present invention at B in FIG. 6;
FIG. 8 is a schematic diagram showing the structure of a process and a system for preparing tri-t-butoxysilanol according to the present invention in a second state;
FIG. 9 is an enlarged schematic view of the process and system for preparing tri-t-butoxysilanol of the present invention at C in FIG. 8;
FIG. 10 is a schematic view showing the structure of a central tube and a first connecting arm of a preparation process and a preparation system of tri-t-butoxysilanol according to the present invention;
FIG. 11 is a schematic diagram of the structure of a first plugging strip and a second plugging strip of a process and a system for preparing tri-t-butoxysilanol according to the present invention;
FIG. 12 is a front view of a process and system for preparing tri-t-butoxysilanol according to the present invention;
FIG. 13 shows the synthesis yield of tri-t-butoxysilanol by a process and system for preparing tri-t-butoxysilanol according to the present invention.
1. A tank body; 2. a stirring shaft; 3. a partition plate; 31. a material leakage hole; 4. a funnel; 41. a flow guiding strip; 5. a boss; 6. a central tube; 7. a polishing section; 71. a first abrasive body; 72. a second abrasive body; 73. a first storage cavity; 75. a movable door; 76. a second storage cavity; 8. a plugging structure; 81. a first connecting arm; 811. a first tension member; 812. a limiting clamp; 82. a second connecting arm; 83. wedge blocks; 84. a first plugging strip; 841. swing arms; 8412. a torsion spring; 85. a rotating sleeve; 851. a shifting block; 86. a second plugging strip; 10. and a second elastic member.
Detailed Description
In order to make the technical scheme of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings.
Referring to fig. 1 to 13, the preparation process of tri-tert-butoxy silanol provided in the embodiment of the present invention includes:
s1, adding n-hexane solvent and sodium tert-butoxide into a tank body 1, and putting the tank body 1 into a normal pressure reflux device to stir by a stirring shaft 2 arranged in the tank body 1;
s2, controlling the heating temperature of the tank body 1 to be a T1 value, adding trichlorosilane into a cavity separated by a partition plate 3 in the tank body 1, adding N-bromosuccinimide raw material into a first storage cavity 73 in the tank body 1, and driving a blocking structure 8 to alternately block the leakage holes 31 when a stirring shaft 2 is stirred at the moment, so that the trichlorosilane liquid raw material quantitatively drops and is dripped through the leakage holes 31, and heating to T2 and keeping reflux for 8 hours after the dripping is finished;
s3, when the stirring shaft 2 drives the blocking structure 8 to control the leakage hole 31 to drop the trichlorosilane, the stirring shaft 2 synchronously drives the grinding part 7 to grind the N-bromosuccinimide raw material, the grinded N-bromosuccinimide powder enters a cavity separated by the partition plate 3 in the tank body 1 and enters the tank body 1 through the leakage hole 31, the temperature is controlled to be T3, the stirring reaction is carried out for 6 hours, and after the stirring is finished, the temperature is controlled to be T4 by adding sodium carbonate and distilled water, and the stirring reaction is carried out for 8 hours;
s4, separating the mixed solution obtained in the step S3 to obtain an organic phase, adding anhydrous sodium sulfate, drying, filtering to obtain a filtrate, removing solvent n-hexane under normal pressure and then reducing pressure, and finally evaporating the crude product of the tri-tert-butoxysilanol under absolute pressure;
and S5, purifying the obtained crude tri-tert-butoxysilanol by vacuum distillation, and removing front and rear fractions according to the proportion of 3-6% of the content of the obtained crude tri-tert-butoxysilanol to obtain a middle fraction which is the finished tri-tert-butoxysilanol product.
Preferably, all of the above S1 to S5 are performed under an inert gas atmosphere, and the n-hexane in the above S1 may be used after drying and water removal.
Preferably, in the above S2, the temperature range of T1 is-10 to 0 ℃, the temperature of T2 is 70 to 75 ℃, and the equivalent ratio of trichlorosilane to sodium tert-butoxide in the above S2 is 1:1.05 to 1.3 times.
Preferably, in the above step S3, the temperature of T3 is in the range of 60to 70 ℃ and the temperature of T4 is 80 ℃.
Preferably, the three-tert-butoxysilanol end product obtained in S5 is subjected to nuclear magnetic resonance and ICP detection by washing with water three times and drying with anhydrous sodium sulfate.
Example 1
Under the protection of inert gas, 1300mL of normal hexane solvent and 604.8g of sodium tert-butoxide are added into a 2L reaction bottle, and a normal pressure reflux device is put on to start stirring;
controlling the temperature of a reaction bottle at-10-0 ℃, dropwise adding 271g of trichlorosilane into the reaction bottle under the protection of inert gas, controlling the speed to be 1-2 drops/s, maintaining stirring for 30min after the dropwise adding is finished, and heating to 70-75 ℃ for reflux for 8h;
adding 375.9g of N-bromosuccinimide after stirring reflux, controlling the temperature to be 60-70 ℃, stirring and reacting for 6 hours, filtering to obtain filtrate after stirring, adding 318g of sodium carbonate and 600mL of distilled water, and stirring and reacting for 8 hours at 80 ℃;
after the stirring reaction is finished, separating the mixed solution to obtain an organic phase, adding 500mL of distilled water for cleaning, separating the solution, repeating the operation for three times, drying the obtained organic phase with anhydrous sodium sulfate, filtering to obtain a filtrate, removing solvent n-hexane under normal pressure and then reducing pressure, and finally evaporating a crude product under absolute pressure;
the obtained crude tri-tert-butoxy silanol is subjected to vacuum rectification and purification: removing the front and rear fractions according to the proportion of 3-6% of the tri-tert-butoxy silanol content, wherein the obtained middle fraction is the tri-tert-butoxy silanol finished product;
the nuclear magnetism and ICP detection of the product are taken;
the synthesis yield of the tri-tert-butoxysilanol in the case is 85%, and the product is confirmed to be the tri-tert-butoxysilanol by detection of a JNM-ECZ400S nuclear magnetic resonance spectrometer; an inductively coupled plasma emission spectrometer (Optima 8000) detects all inorganic elements <1ppm, with a purity of up to 6N.
Example two
Under the protection of inert gas, 1300mL of normal hexane solvent and 633.6g of sodium tert-butoxide are added into a 2L reaction bottle, and a normal pressure reflux device is put on to start stirring;
controlling the temperature of a reaction bottle at-10-0 ℃, dropwise adding 271g of trichlorosilane into the reaction bottle under the protection of inert gas, controlling the speed to be 1-2 drops/s, maintaining stirring for 30min after the dropwise adding is finished, and heating to 70-75 ℃ for reflux for 8h;
adding 375.9g of N-bromosuccinimide after stirring reflux, controlling the temperature to be 60-70 ℃, stirring and reacting for 6 hours, filtering to obtain filtrate after stirring, adding 318g of sodium carbonate and 600mL of distilled water, and stirring and reacting for 8 hours at 80 ℃;
after the stirring reaction is finished, separating the mixed solution to obtain an organic phase, adding 500mL of distilled water for cleaning, separating the solution, repeating the operation for three times, drying the obtained organic phase with anhydrous sodium sulfate, filtering to obtain a filtrate, removing solvent n-hexane under normal pressure and then reducing pressure, and finally evaporating a crude product under absolute pressure;
the obtained crude tri-tert-butoxy silanol is subjected to vacuum rectification and purification: removing the front and rear fractions according to the proportion of 3-6% of the tri-tert-butoxy silanol content, wherein the obtained middle fraction is the tri-tert-butoxy silanol finished product;
the nuclear magnetism and ICP detection of the product are taken;
the synthesis yield of the tri-tert-butoxysilanol in the case is 88.3%, and the product is confirmed to be tri-tert-butoxysilanol by detection of a JNM-ECZ400S nuclear magnetic resonance spectrometer; the inductively coupled plasma emission spectrum (Optima 8000) detects all inorganic elements <1ppm, with a purity of up to 6N.
Example III
Under the protection of inert gas, 1300mL of normal hexane solvent and 691.2g of sodium tert-butoxide are added into a 2L reaction bottle, and a normal pressure reflux device is put on to start stirring;
controlling the temperature of a reaction bottle at-10-0 ℃, dropwise adding 271g of trichlorosilane into the reaction bottle under the protection of inert gas, controlling the speed to be 1-2 drops/s, maintaining stirring for 30min after the dropwise adding is finished, and heating to 70-75 ℃ for reflux for 8h;
adding 375.9g of N-bromosuccinimide after stirring reflux, controlling the temperature to be 60-70 ℃, stirring and reacting for 6 hours, filtering to obtain filtrate after stirring, adding 318g of sodium carbonate and 600mL of distilled water, and stirring and reacting for 8 hours at 80 ℃;
after the stirring reaction is finished, separating the mixed solution to obtain an organic phase, adding 500mL of distilled water for cleaning, separating the solution, repeating the operation for three times, drying the obtained organic phase with anhydrous sodium sulfate, filtering to obtain a filtrate, removing solvent n-hexane under normal pressure and then reducing pressure, and finally evaporating a crude product under absolute pressure;
the obtained crude tri-tert-butoxy silanol is subjected to vacuum rectification and purification: removing the front and rear fractions according to the proportion of 3-6% of the tri-tert-butoxy silanol content, wherein the obtained middle fraction is the tri-tert-butoxy silanol finished product;
the nuclear magnetism and ICP detection of the product are taken;
the synthesis yield of the tri-tert-butoxysilanol in the case is 88.5%, and the product is confirmed to be tri-tert-butoxysilanol by detection of a JNM-ECZ400S nuclear magnetic resonance spectrometer; the inductively coupled plasma emission spectrum (Optima 8000) detects all inorganic elements <1ppm, with a purity of up to 6N.
Example IV
Under the protection of inert gas, 1300mL of normal hexane solvent and 748.8g of sodium tert-butoxide are added into a 2L reaction bottle, and a normal pressure reflux device is put on to start stirring;
controlling the temperature of a reaction bottle at-10-0 ℃, dropwise adding 271g of trichlorosilane into the reaction bottle under the protection of inert gas, controlling the speed to be 1-2 drops/s, maintaining stirring for 30min after the dropwise adding is finished, and heating to 70-75 ℃ for reflux for 8h;
adding 375.9g of N-bromosuccinimide after stirring reflux, controlling the temperature to be 60-70 ℃, stirring and reacting for 6 hours, filtering to obtain filtrate after stirring, adding 318g of sodium carbonate and 600mL of distilled water, and stirring and reacting for 8 hours at 80 ℃;
after the stirring reaction is finished, separating the mixed solution to obtain an organic phase, adding 500mL of distilled water for cleaning, separating the solution, repeating the operation for three times, drying the obtained organic phase with anhydrous sodium sulfate, filtering to obtain a filtrate, removing solvent n-hexane under normal pressure and then reducing pressure, and finally evaporating a crude product under absolute pressure;
the obtained crude tri-tert-butoxy silanol is subjected to vacuum rectification and purification: removing the front and rear fractions according to the proportion of 3-6% of the tri-tert-butoxy silanol content, wherein the obtained middle fraction is the tri-tert-butoxy silanol finished product;
the nuclear magnetism and ICP detection of the product are taken;
the synthesis yield of the tri-tert-butoxysilanol in the case is 88.5%, and the product is confirmed to be tri-tert-butoxysilanol by detection of a JNM-ECZ400S nuclear magnetic resonance spectrometer; an inductively coupled plasma emission spectrometer (Optima 8000) detects all inorganic elements <1ppm, with a purity of up to 6N.
In the four examples described above, in step S2, the equivalent ratio of trichlorosilane to sodium tert-butoxide was 1:1.05 to 1.3 times, wherein the reaction of sodium tert-butoxide and trichlorosilane is 3 to 1, and in the embodiment, the equivalent ratio of the trichlorosilane to the sodium tert-butoxide is 1:1.05 to 1.3, namely equivalent (eq) ratio, which is to multiply 3 according to mole ratio, should be 1: 3.14-3.9.
In the step S4, the normal pressure is 760Torr, most of the normal hexane solvent is distilled off at normal pressure, the pressure is controlled to be 10Torr under normal temperature to remove the rest normal hexane solvent, and the absolute pressure is controlled to be 5Torr at 100-120 ℃ to distill out the crude product.
Referring to fig. 13, in the above examples, the amount of sodium tert-butoxide is gradually increased in the four examples, and in the third example, 691.2g of sodium tert-butoxide is added to 1300mL of n-hexane solvent, so as to ensure that the equivalent ratio of trichlorosilane to sodium tert-butoxide is 1:1.1, the synthesis yield of the tri-tert-butoxyl silanol is highest and the used raw materials are the least, and the synthesis method has the advantages of simple process, few reaction steps, reasonable raw material proportion and less waste generation, so that the cost of raw materials for preparation is reduced, the equipment investment cost and the subsequent preparation cost can be effectively reduced in the industrialized promotion, and the energy-saving and environment-friendly production concept is met.
In the steps S2-S3, trichlorosilane is required to be dropwise added into a reaction container, the trichlorosilane has high reactivity, the reaction is usually severe and needs careful treatment, the reaction intensity is reduced by adopting a mode of lengthening the adding time, if the trichlorosilane is intensively added, a great amount of trichlorosilane is intensively reacted, the local temperature in the reaction container is excessively increased instantly, the boiling point of the trichlorosilane is 32-34 ℃, the trichlorosilane is gasified once the temperature is increased, the reaction cannot be smoothly carried out, in the step S3, N-bromosuccinimide needs to be added into the reaction container and is stirred for 6h, the N-bromosuccinimide is crystalline, the solution reaction is slow, and the synthesis speed is further reduced, so in order to accelerate the reaction speed, a preparation system of the following preparation system, in particular, a preparation system of tri-tert-butoxysilanol is provided, which comprises a tank body 1, a stirring shaft 2 is arranged in the tank body 1, and the steps are further included:
a polishing section 7;
the central tube 6 is movably inserted into the tank body 1, and after solid raw materials are added into the grinding part 7, the central tube 6 receives the transmission of the stirring shaft 2 so as to drive the grinding part 7 to crush the raw materials through the central tube 6;
the separation plate 3 is arranged in the tank body 1, a plurality of material leakage holes 31 are uniformly formed in the separation plate 3, and liquid raw materials are contained above the separation plate 3;
the plugging structure 8 is arranged on the central tube 6, and according to different rotation speeds of the stirring shaft 2, the corresponding plugging structure 8 is provided with a first state and a second state, the plugging structure 8 alternately plugs the upper end and the lower end of the material leakage hole 31 in the first state, liquid raw materials quantitatively fall through the material leakage hole 31, the grinding part 7 is passively opened in the second state, and solid raw materials in the grinding part 7 fall through the material leakage hole 31.
The lower part of the tank body 1 is used as a reaction area, the reaction area at the lower part of the tank body 1 can be stirred through the stirring shaft 2 so as to promote the reaction, the upper part of the central tube 6 is provided with a second elastic piece 10, an upward thrust is applied to the central tube 6 through the second elastic piece 10, after N-bromosuccinimide is added to the grinding part 7, the mass of the grinding part 7 is increased, the central tube 6 resists the thrust of the second elastic piece 10, the central tube 6 is lowered in the vertical direction, and the lower end of the central tube 6 is in transmission connection with the stirring shaft 2 after the central tube 6 is lowered in the height, so that the central tube 6 is synchronously driven to rotate correspondingly in the stirring process of the stirring shaft 2;
the lower part of the central tube 6 is set to be in a sealed state, the upper part of the central tube 6 is connected with a liquid inlet pipeline, so that the added trichlorosilane liquid can be conveyed through the central tube 6, and can enter the partition plate 3 through the conveying of the central tube 6, and the trichlorosilane is intercepted through the partition plate 3, so that the trichlorosilane is intercepted in a cavity at the upper part of the tank body 1 and cannot enter the lower part of the tank body 1, the trichlorosilane is prevented from contacting the solution obtained in the S1, a plurality of leaking holes 31 are formed in the partition plate 3, and the trichlorosilane can only flow to the lower part of the tank body 1 through the leaking holes 31;
the plugging structure 8 can rotate along with the central pipe, the plugging structure 8 is used for alternatively plugging the material leakage holes 31 in the rotating process, when the lower part of the material leakage holes 31 is plugged, the opening at the upper part of the material leakage holes 31 is in an open state, the trichlorosilane intercepted by the partition plate 3 flows into the material leakage holes 31, the opening at the upper part of the material leakage holes 31 is plugged along with the rotating process, the opening at the lower part of the material leakage holes 31 is opened, the trichlorosilane existing in the material leakage holes 31 can fall into the lower part of the tank body 1, the trichlorosilane contacts with the solution obtained by the S1 and reacts, the material leakage holes 31 are uniformly distributed in the tank body 1, so that the trichlorosilane existing in each material leakage hole 31 can uniformly fall into the lower part of the tank body 1, the effect of dispersing the trichlorosilane is achieved, the trichlorosilane is concentrated in a certain area of the tank body 1, the problem that the solution in the tank body 1 is locally excessively high to cause the trichlorosilane to vaporize the bromosilane is solved, the bromosuccinimide is remarkably increased, the bromosuccinimide is added into the reaction tank body 1, the bromosuccinimide is grinded in the reaction area by the reaction area of the 3-7, the bromosuccinimide is grinded in the reaction area, the reaction area is reduced, the bromosuccinimide is grinded in the reaction area of the reaction area is reduced, and the reaction area is the bromosuccinimide is grinded in the reaction area is 7, and the reaction area is reduced by the reaction area, and the bromosuccinimide is added in the reaction area is completely, and the reaction area is grinded in the area is reduced by the reaction area, and the reaction area is 3, by decelerating the stirring shaft 2, and leaving the grinding part 7 in the idle position, the central tube 6 can be disconnected from the stirring shaft 2, so that the load of the stirring shaft 2 is reduced. The step addition of the trichlorosilane and the N-bromosuccinimide can be realized only by adjusting the speed of the stirring shaft 2, and after the addition is finished, the central tube 6 and the stirring shaft 2 are disconnected.
Referring to fig. 2 to 4, the grinding portion 7 includes a first grinding body 71, a second grinding body 72 and a movable door 75, the first grinding body 71 is fixedly installed on an upper portion of an inner wall of the tank 1, a first storage cavity 73 is provided on an upper portion of the first grinding body 71, the second grinding body 72 is fixedly installed on an outer portion of the central tube 6, a second storage cavity 76 is provided on lower portions of the first grinding body 71 and the second grinding body 72, the movable door 75 is provided on a lower portion of the first grinding body 71, the movable door 75 seals the second storage cavity 76 in a first state, and the movable door 75 is opened in a second state.
The first grinding body 71 and the tank body 1 are concentric, the central tube 6 is also arranged on the central line of the tank body 1, the second grinding body 72 is fixed outside the central tube 6, so that the tank body 1, the central tube 6, the first grinding body 71 and the second grinding body 72 are positioned on the same concentric line, the first storage cavity 73 is used for storing N-bromosuccinimide, after the N-bromosuccinimide is added through a feeding pipe at the upper part of the tank body 1, the mass of the second grinding body 72 is increased, the central tube 6 moves downwards under the pressure of the N-bromosuccinimide and the second grinding body 72, the central tube 6 and the stirring shaft 2 are coaxial, the central tube 6 is sleeved at the upper part of the stirring shaft 2, the second grinding body 72 can be driven to rotate through the rotation of the stirring shaft 2, the raw materials in the first storage cavity 73 enter the first grinding body 71 and the second grinding body, the N-bromosuccinimide enters the separation plate 31 in the gap between the first grinding body 71 and the second grinding body, the N-bromosuccinimide enters the separation plate 75 in the gap between the second grinding body and the second grinding body 72, the N-bromosuccinimide is opened, the N-bromosuccinimide enters the separation plate 75 in the gap between the tank body and the gap is opened, and the N-bromosuccinimide is opened at the bottom of the gap between the N-bromosuccinimide and the second grinding body is opened, and the N-bromosuccinimide is more, and the N-bromosuccinimide is opened, and the crystal is moved in the gap between the second grinding material is in the gap between the second grinding material and the second grinding material is in the second grinding material and the second grinding material.
Referring to fig. 4, a funnel 4 is provided at an upper portion of the separation plate 3, a boss 5 is provided at a central upper portion of the separation plate 3, and a discharge hole 31 is provided between the funnel 4 and the boss 5.
The funnel 4 is gradually lowered from the periphery to the middle part, the middle part is matched with the funnel 4 by arranging the protruding table 5, an accommodating space can be just formed between the protruding table 5 and the funnel 4, N-bromosuccinimide can firstly fall on the funnel 4 after being separated from the grinding part 7, N-bromosuccinimide is collected through the inclined plane of the funnel 4, and therefore the N-bromosuccinimide can conveniently fall to the lower part of the tank body 1 through the material leakage hole 31.
Referring to fig. 6-9 and 11, the plugging structure 8 includes a first connecting arm 81, a first tension member 811, a second connecting arm 82, a first plugging bar 84, a rotating sleeve 85 and a second plugging bar 86, the first connecting arm 81 is slidably inserted on the central tube 6, the second connecting arm 82 is slidably sleeved on the first connecting arm 81, the first tension member 811 applies a tension force towards the central tube 6 to the second connecting arm 82, a swing arm 841 is fixedly connected to the first plugging bar 84, the upper end of the swing arm 841 is connected to the second connecting arm 82, the rotating sleeve 85 is rotatably connected to the lower portion of the partition plate 3, the rotating sleeve 85 is connected with the central tube 6 through a transmission portion, and the second plugging bar 86 is fixedly mounted outside the rotating sleeve 85.
The central tube 6 is provided with a notch, the first connecting arm 81 penetrates through the notch, the end part of the first connecting arm 81 is provided with a limiting clamp 812, the limiting clamp 812 is in sliding connection with the central tube 6, the position of the first connecting arm 81 can be limited through the limiting clamp 812, the first connecting arm 81 is prevented from being separated from the central tube 6, the central tube 6 can be ensured to be capable of changing in height in the vertical direction, the second connecting arm 82 is in sliding connection with the first connecting arm 81, when the central tube 6 rotates, the first connecting arm 81 and the second connecting arm 82 can be driven to synchronously rotate, one end of the first tensile member 811 is arranged on the second connecting arm 82, the other end of the first tensile member 811 is arranged on the limiting clamp 812, and in the first state, the first tensile member 811 applies a tensile force to the second connecting arm 82, so that the second connecting arm 82 keeps a relative static state between the first connecting arm 81 and the second connecting arm 82 in the rotating process, the first blocking strip 84 is just positioned between the funnel 4 and the boss 5, the first blocking strip 84 is positioned through the funnel 4 and the boss 5to keep a horizontal state, in the rotation process of the central tube 6, the first blocking strip 84 rotates synchronously through the connection effect of the swing arm 841, the shape path of the first blocking strip 84 covers the upper opening of the leaking hole 31, in the rotation process of the first blocking strip 84, the sealing and opening of the upper part of the leaking hole 31 can be realized, in the opening process, trichlorosilane can be poured into the leaking hole 31, the rotating sleeve 85 is connected in the partition plate 3 in a rotating way, the rotating sleeve 85 is coaxial with the central tube 6, the transmission part comprises a shifting block 851, the shifting block 851 is fixedly arranged outside the central tube 6, a sliding groove is formed on the rotating sleeve 85, one end of the shifting block 851 is inserted into the sliding groove, the chute is reserved with a certain margin when being opened in the vertical direction, so that the chute can not interfere with the displacement of the shifting block 851 in the vertical direction when the height of the central tube 6 is changed, the central tube 6 can synchronously rotate through the arrangement of the transmission part, the second sealing strip 86 is driven to rotate when the rotating sleeve 85 rotates, the lower surface of the second sealing strip 86 and the lower surface of the partition plate 3 are attached, the lower opening of the material leakage hole 31 is covered by the rotating path of the second sealing strip 86, and thus, in the rotating process of the second sealing strip 86, the lower part of the material leakage hole 31 can have two states, and the sealing and the opening are carried out, when the sealing strip is opened, the stored trichlorosilane in the material leakage hole 31 can fall into the reaction cavity of the lower part of the tank body 1, the first sealing strip 84 and the second sealing strip 86 need to be staggered, when the upper opening of the material leakage hole 31 is sealed, the lower part needs to be sealed, thus, the trichlorosilane isolated by the partition plate 3 enters the reaction tank body 1, and the trichlorosilane is prevented from entering the high-volume and the high-volume trichlorosilane is prevented from entering the reaction tank 1.
Referring to fig. 5to 6, a wedge 83 is fixedly installed at one end of the second connecting arm 82, and in a first state, the wedge 83 abuts against a lower portion of the movable door 75, and in a second state, a contact point between the wedge 83 and the movable door 75 moves downward. In S2, when adding N-bromosuccinimide is needed after adding trichlorosilane is completed, the rotation speed of the stirring shaft 2 is increased, so that the rotation speed of the central tube 6 is synchronously increased, the second connecting arm 82 is acted by centrifugal force, the second connecting arm 82 resists the pulling force of the first pulling member 811, the second connecting arm 82 stretches out, the wedge 83 arranged at the end of the second connecting arm 82 is synchronously displaced, the wedge 83 is displaced in a direction away from the central tube 6, so that the contact point between the wedge 83 and the movable door 75 is changed, the upper surface of the wedge 83 is an inclined plane, the height of the movable door 75 is reduced, the N-bromosuccinimide arranged in the second storage cavity 76 is separated, the N-bromosuccinimide enters the funnel 4, and finally enters the lower reaction area of the tank 1 from the leak hole 31.
In still another embodiment of the present invention, referring to fig. 9, in the second state, the movable door 75 is opened, the N-bromosuccinimide moves along the funnel 4, the guide strip 41 is disposed on the inclined surface of the funnel 4, the N-bromosuccinimide moves along the middle portion of the guide strip 41 along the partition plate 3, so that the N-bromosuccinimide better falls down to the leak hole 31, the swing arm 841 is rotatably connected to the second connecting arm 82, the swing arm 841 is provided with the torsion spring 8412, after the second connecting arm 82 moves transversely, the swing arm 841 swings, and the first sealing strip 84 is turned synchronously, so that the first sealing strip 84 is completely separated from the leak hole 31, thereby facilitating the entry of the N-bromosuccinimide, and at this time, the first sealing strip 84 plays a stirring role, so as to avoid the accumulation on the partition plate 3 in the N-bromosuccinimide, ensure the smooth funnel of the leak, and at the final stage, only a very small portion of the N-bromosuccinimide of the 4 remains on the funnel, and the first sealing strip 84 is reciprocally driven by the first sealing strip 84, and the first sealing strip 84 is reciprocally vibrated by the first sealing strip 84, so that the N-bromosuccinimide is reciprocally attached to the funnel 84, and the first sealing strip 84 is reciprocally moved by the first sealing strip 4.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that modifications may be made to the described embodiments in various different ways without departing from the spirit and scope of the invention. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive of the scope of the invention, which is defined by the appended claims.
Claims (7)
1. A process for preparing tri-t-butoxysilanol comprising:
s1, adding n-hexane solvent and sodium tert-butoxide into a tank body (1), and putting the tank body into a normal pressure reflux device to stir by a stirring shaft (2) arranged in the tank body (1);
s2, controlling the heating temperature of the tank body (1) at a value T1, adding trichlorosilane into a cavity separated by a partition plate (3) in the tank body (1), adding N-bromosuccinimide raw material into a first material storage cavity (73) in the tank body (1), wherein a material leakage hole (31) is formed in the partition plate (3), and driving a blocking structure (8) to alternately block the material leakage hole (31) when a stirring shaft (2) is used for stirring, so that the trichlorosilane liquid raw material quantitatively drops and is dripped through the material leakage hole (31), and heating to T2 and keeping reflux for 8 hours after the dripping is finished;
s3, when the stirring shaft (2) drives the blocking structure (8) to control the leakage hole (31) to drop the trichlorosilane, the stirring shaft (2) synchronously drives the grinding part (7) to grind the N-bromosuccinimide raw material, the grinded N-bromosuccinimide powder enters a cavity separated by the partition plate (3) in the tank body (1) and enters the tank body (1) through the leakage hole (31), the temperature is controlled to be T3, the stirring reaction is carried out for 6 hours, and after the stirring is finished, sodium carbonate and distilled water are added to control the temperature to be T4, and the stirring reaction is carried out for 8 hours;
s4, separating the mixed solution obtained in S3 to obtain an organic phase, adding anhydrous sodium sulfate, drying, filtering to obtain a filtrate, removing normal hexane as a solvent under normal pressure and then reducing pressure, and finally, evaporating a crude product of tri-tert-butoxysilanol under absolute pressure, wherein the absolute pressure is that the pressure is controlled to be 5Torr, and the temperature is 100-120 ℃ to evaporate the crude product;
and S5, purifying the obtained crude tri-tert-butoxysilanol by vacuum distillation, and removing front and rear fractions according to the proportion of 3-6% of the content of the obtained crude tri-tert-butoxysilanol to obtain a middle fraction which is a finished tri-tert-butoxysilanol product.
2. The process for preparing tri-t-butoxysilanol according to claim 1, wherein S1 to S5 are carried out under an inert gas atmosphere, and n-hexane in S1 is used after drying and water removal.
3. The process for preparing tri-tert-butoxysilanol according to claim 1, wherein in S2, T1 is at a temperature ranging from-10 to 0 ℃ and T2 is at a temperature ranging from 70 to 75 ℃, and the molar ratio of trichlorosilane to sodium tert-butoxide in S2 is 1: 3.14-3.9.
4. The process according to claim 1, wherein in S3, T3 is at a temperature ranging from 60to 70 ℃ and T4 is at a temperature of 80 ℃.
5. The process for preparing tri-t-butoxysilanol according to claim 1, wherein the liquid separation in S4 is performed by washing with water three times and then drying with anhydrous sodium sulfate, and the tri-t-butoxysilanol product obtained in S5 is subjected to nuclear magnetic resonance detection and ICP detection.
6. A device for preparing tri-tert-butoxysilanol, which is used for realizing the tri-tert-butoxysilanol preparing process according to any one of claims 1 to 5, further comprising a tank (1), wherein a stirring shaft (2) is provided in the tank (1), further comprising:
a polishing section (7);
the central tube (6) is movably inserted into the tank body (1), and after solid raw materials are added into the grinding part (7), the central tube (6) receives the transmission of the stirring shaft (2) so as to drive the grinding part (7) to crush the raw materials through the central tube (6);
the separation plate (3) is arranged in the tank body (1), a plurality of leakage holes (31) are uniformly formed in the separation plate (3), and liquid raw materials are contained above the separation plate (3);
the blocking structure (8) is arranged on the central tube (6), and corresponds to the different rotation speeds of the stirring shaft (2), the blocking structure (8) is provided with a first state and a second state, the blocking structure (8) alternately blocks the upper end and the lower end of the material leakage hole (31) in the first state, liquid raw materials quantitatively fall through the material leakage hole (31), the grinding part (7) is passively opened in the second state, and solid raw materials in the grinding part (7) fall through the material leakage hole (31);
the grinding part (7) comprises a first grinding body (71), a second grinding body (72) and a movable door (75), wherein the first grinding body (71) is fixedly arranged on the upper portion of the inner wall of the tank body (1), a first storage cavity (73) is formed in the upper portion of the first grinding body (71), the second grinding body (72) is fixedly arranged outside the central tube (6), a second storage cavity (76) is formed in the lower portions of the first grinding body (71) and the second grinding body (72), the movable door (75) is arranged on the lower portion of the first grinding body (71), the movable door (75) is used for sealing the second storage cavity (76) in a first state, and the movable door (75) is opened in a second state;
the plugging structure (8) comprises a first connecting arm (81), a first tension piece (811), a second connecting arm (82), a first plugging strip (84), a rotary sleeve (85) and a second plugging strip (86), wherein the first connecting arm (81) is in sliding connection with the central tube (6), the second connecting arm (82) is in sliding connection with the first connecting arm (81), the first tension piece (811) applies a tension towards the central tube (6) to the second connecting arm (82), a swing arm (841) is fixedly connected to the first plugging strip (84), the upper end of the swing arm (841) is connected to the second connecting arm (82), the rotary sleeve (85) is in rotary connection with the lower part of the partition plate (3), the rotary sleeve (85) is connected with the central tube (6) through a transmission part, and the second plugging strip (86) is fixedly arranged outside the rotary sleeve (85);
one end of the second connecting arm (82) is fixedly provided with a wedge block (83), in a first state, the wedge block (83) is abutted against the lower part of the movable door (75), and in a second state, the contact point of the wedge block (83) and the movable door (75) moves downwards.
7. The apparatus for producing tri-t-butoxysilanol according to claim 6, wherein a funnel (4) is provided at an upper portion of the partition plate (3), a boss (5) is provided at a central upper portion of the partition plate (3), and the position of the weeping hole (31) is provided between the funnel (4) and the boss (5).
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB656774A (en) * | 1942-12-31 | 1951-09-05 | Minnesota Mining & Mfg | Improvements in or relating to processes of preparing new organic silicon compounds and the compounds resulting from said process |
| US3310578A (en) * | 1963-12-20 | 1967-03-21 | Gen Electric | Substituted silanes |
| CN211660718U (en) * | 2019-12-13 | 2020-10-13 | 四川企易标信息科技有限公司 | Dissolving device for polyethylene recovery |
| CN113755305A (en) * | 2021-10-19 | 2021-12-07 | 云南星桥食品有限公司 | Method and equipment for processing rice noodles by microbial treatment |
| CN216272070U (en) * | 2021-12-10 | 2022-04-12 | 山东滨州智源生物科技有限公司 | Hydroxypropyl gamma cyclodextrin feeding device |
| CN115248314A (en) * | 2022-01-12 | 2022-10-28 | 赵华 | Blood sugar detection device for endocrinology department |
| CN116284096A (en) * | 2023-05-19 | 2023-06-23 | 研峰科技(北京)有限公司 | Synthesis method of tri (tert-butoxy) silanol with ultralow chloride ion content |
-
2024
- 2024-01-09 CN CN202410027054.0A patent/CN117534697B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB656774A (en) * | 1942-12-31 | 1951-09-05 | Minnesota Mining & Mfg | Improvements in or relating to processes of preparing new organic silicon compounds and the compounds resulting from said process |
| US3310578A (en) * | 1963-12-20 | 1967-03-21 | Gen Electric | Substituted silanes |
| CN211660718U (en) * | 2019-12-13 | 2020-10-13 | 四川企易标信息科技有限公司 | Dissolving device for polyethylene recovery |
| CN113755305A (en) * | 2021-10-19 | 2021-12-07 | 云南星桥食品有限公司 | Method and equipment for processing rice noodles by microbial treatment |
| CN216272070U (en) * | 2021-12-10 | 2022-04-12 | 山东滨州智源生物科技有限公司 | Hydroxypropyl gamma cyclodextrin feeding device |
| CN115248314A (en) * | 2022-01-12 | 2022-10-28 | 赵华 | Blood sugar detection device for endocrinology department |
| CN116284096A (en) * | 2023-05-19 | 2023-06-23 | 研峰科技(北京)有限公司 | Synthesis method of tri (tert-butoxy) silanol with ultralow chloride ion content |
Non-Patent Citations (2)
| Title |
|---|
| tert-Butoxysilanols as model comounds for labile key intermediates of the sol-gel process：crystal and molecular structures of (t-BuO)3SiOH and HO((t-BuO)2SiO)2H;Jens Beckmann等;《APPLIED ORGANOMENTALIC CHEMISTRY》;20021206;第17卷;第52-62页 * |
| 三叔丁氧基氢化铝锂的新型制备方法;车瀛照;;天津化工;20171130(06);全文 * |
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