CN110563953A - Preparation method of silicone oil - Google Patents
Preparation method of silicone oil Download PDFInfo
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- CN110563953A CN110563953A CN201910906672.1A CN201910906672A CN110563953A CN 110563953 A CN110563953 A CN 110563953A CN 201910906672 A CN201910906672 A CN 201910906672A CN 110563953 A CN110563953 A CN 110563953A
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- water
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- kettle body
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- 229920002545 silicone oil Polymers 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 117
- 238000007599 discharging Methods 0.000 claims abstract description 70
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- 238000005507 spraying Methods 0.000 claims abstract description 38
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000007921 spray Substances 0.000 claims abstract description 35
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 32
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 32
- 238000009835 boiling Methods 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 238000006136 alcoholysis reaction Methods 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims abstract description 19
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 19
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- 239000003921 oil Substances 0.000 claims abstract description 10
- 239000006184 cosolvent Substances 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- 230000032798 delamination Effects 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 24
- 238000001125 extrusion Methods 0.000 claims description 7
- 230000003472 neutralizing effect Effects 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 28
- 239000007788 liquid Substances 0.000 description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 19
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 19
- 239000007864 aqueous solution Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000000413 hydrolysate Substances 0.000 description 2
- -1 sulfate ester Chemical class 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/10—Equilibration processes
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention belongs to the technical field of preparation of silicone oil, and particularly relates to a preparation method of silicone oil; the method comprises the following steps: s1: the raw material ratio is as follows: 100 parts by weight of organosilicon high-boiling residues; 30-40 parts by weight of methanol; 15-18 parts of methanol cosolvent and equal amount of urea; 1.0-1.5 parts of ammonia water; s2: alcoholysis: adding 100 parts by weight of organic silicon high-boiling residues into the reaction kettle body through a feeding pipe, and dropwise adding 30-40 parts by weight of methanol; filtering the crude high-boiling silicon oil obtained by neutralization and delamination in the step S3 through a discharging box arranged in the reaction kettle body, filtering acid water and impurities, and discharging through a discharging pipe; a spraying device arranged in the reaction kettle body sprays water to absorb hydrogen chloride gas generated in the alcoholysis process; 0.2-0.5 part of ammonia water is mixed in the water solution of the spraying device; the hydrochloric acid can be subjected to neutralization reaction by evaporating ammonia water with weight percentage lower than that of the hydrochloric acid, so that the addition amount of the ammonia water during neutralization is reduced, and the neutralization speed of the high-boiling-point silicon oil is increased.
Description
Technical Field
The invention belongs to the technical field of preparation of silicone oil, and particularly relates to a preparation method of silicone oil.
background
Organosilicon is an important emerging material and has wide application in many fields. With the rapid development of the organosilicon industry, a large amount of silane high-boiling residues are generated in the process of synthesizing organosilicon monomer methyl chlorosilane.
The preparation of the silicone oil by the traditional method is that the organic silicon high-boiling residue is put into a reaction kettle, absolute methanol is added for alcoholysis reaction, and the temperature is raised to drive acid for h; adding 2 times of solvent and 4 times of water into the alcoholysis product, performing hydrolysis reaction, standing to separate acid water after reaction, washing the upper layer product to be neutral, and performing reduced pressure distillation to obtain hydrolysate; mixing the hydrolysate with MM and catalyst, stirring for equilibrium reaction, separating out sulfate, washing the product to neutrality, drying, and filtering to obtain the target product.
In the method, when the silicone oil is prepared, in the steps after alcoholysis and before neutralization, an aqueous solution is sprayed into a reaction kettle to absorb hydrogen chloride gas generated after alcoholysis; most of the aqueous solutions are sprayed into the kettle body through the high-pressure spray head, the efficiency of the aqueous solutions for absorbing hydrogen chloride gas is easily reduced when the aqueous solutions are sprayed, the proportion of ammonia water used in neutralization is increased, and a large amount of ammonia water needs to be added for neutralization reaction in the neutralization step.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides the preparation method of the silicone oil, which is mainly used for solving the problem that most of the existing aqueous solutions are sprayed into a kettle body through a high-pressure spray head, the efficiency of absorbing hydrogen chloride gas by the aqueous solutions is easily reduced when the aqueous solutions are sprayed, the proportion of using ammonia water during neutralization is increased, and a large amount of ammonia water needs to be added for neutralization reaction during the neutralization step.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the silicone oil comprises the following steps:
S1: the raw material ratio is as follows: 100 parts by weight of organosilicon high-boiling residues; 30-40 parts by weight of 80-90% by weight of raw material methanol; 15-18 parts of methanol cosolvent and equal amount of urea; 1.0-1.5 parts of 27% ammonia water by weight;
S2: alcoholysis: adding 100 parts by weight of organic silicon high-boiling residues into a reaction kettle body through a feeding pipe at the temperature of between 20 and 25 ℃, dropwise adding 30 to 40 parts by weight of raw material methanol with the weight percentage of between 80 and 90 percent for 6 to 8 hours; the initial dropping speed is 3 parts/hour, and the dropping time is 2-3 hours; gradually extracting to 10 parts/hour;
S3: neutralizing: adding 15-18 parts of methanol cosolvent and equal amount of urea into the materials at normal temperature, wherein the neutralization temperature is 42-50 ℃, and the neutralization time is 0.5 hour, so as to neutralize hydrochloric acid in the materials; layering to obtain crude high-boiling-point silicone oil with the pH value of 4-5, adding 0.7-1.0 part of 27% ammonia water by weight, and continuously neutralizing to ensure that the pH value is 6-8;
S4: and (3) filtering: and (3) filtering the crude high-boiling silicon oil obtained by neutralization and delamination in the step S3 through a discharge box arranged in the reaction kettle body, and discharging filtered acid water and impurities through a discharge pipe.
Preferably, the step of S3 further comprises deacidifying; deacidifying: the temperature of the reaction kettle body rises to 45-60 ℃; a spraying device arranged in the reaction kettle body sprays water to absorb hydrogen chloride gas generated in the alcoholysis process; 0.2-0.5 part of 30% ammonia water in percentage by weight is mixed in the water solution of the spraying device; the setting through spray set can absorb the aqueous solution that sprays through the aqueous solution that produces after the internal alcoholysis of reation kettle, the aqueous solution of 30% weight percent's of the aqueous solution of interpolation aqueous solution can evaporate the production ammonia in the environment of reation kettle body high temperature simultaneously, ammonia and aqueous ammonia solution can react with the hydrogen chloride gas, the weight percent aqueous ammonia after the evaporation simultaneously is less than 30% weight percent's aqueous ammonia, aqueous ammonia after the evaporation can carry out neutralization reaction with hydrochloric acid, and then the addition of aqueous ammonia when having reduced the neutralization, accelerate the neutralization speed of high boiling silicone oil simultaneously.
Preferably, a discharging box is arranged in the reverse kettle body in a swinging mode through a rubber swinging column, the upper end of the bottom end of the discharging box is in an open state, and a sealing disc is arranged at the bottom end of the discharging box in a sliding mode; the sealing disc is connected with the telescopic end of the electric telescopic rod through the rubber soft column, and the bottom end of the electric telescopic rod is fixed at the bottom end of the reaction kettle body; a plurality of filter screen plates are arranged on the side wall of the upper end of the discharging box, and the thickness of each filter screen plate is larger than that of the discharging box; when the device works, raw materials are put into a material discharging box through a feeding pipe, crude high-boiling silicone oil is obtained through alcoholysis, acid washing and neutralization steps, after the crude high-boiling silicone oil and neutral product water and sulfate are layered, a control unit controls an electric telescopic rod to extend out, the electric telescopic rod drives a sealing disc to slide upwards in the material discharging box, so that silicone oil and product water in the material discharging box are pushed upwards after the layers are layered, after the neutralized product water and the sulfate move upwards to the position of a filter screen plate, the filter screen plate can filter and discharge the produced water and the sulfate out of the material discharging box along with the continuous upward movement of the sealing disc, the product water and the sulfate discharged from the material discharging box can be discharged through a discharging pipe arranged at the bottom end of a reaction kettle body, and after the product water and the sulfate are cleaned, an operator cleans the bottom end of the reaction kettle body and the discharging pipe; simultaneously, the silicone oil after filtering can drive the sealing disc to move downwards through the electric telescopic rod, the sealing disc can be opened from the bottom end of the discharging box, and then the high-boiling silicone oil is discharged from a discharging port at the bottom end of the reaction kettle body.
Preferably, the spraying device comprises a driving motor, a rotating screw rod, a rotating disc, a water guide pipe, a cavity rotating column and a water spraying pipe; the driving motor is installed at the top end of the reaction kettle body, and the output end of the driving motor penetrates through the reaction kettle body and is connected with the rotating screw rod; the rotating screw rod is rotatably connected with a rotating disc through a ball nut pair, and the upper surface of the rotating disc is provided with a rotating groove; a concave groove is formed in the side face of the rotating disc, and a plurality of water spray pipes are arranged in the concave groove in a swinging mode through the cavity rotating column; the two side walls of the water spraying pipe are provided with water spraying holes, and the end parts of the water spraying holes are provided with filter net films; the water spraying pipe is communicated with the cavity rotating column; one end of the water guide pipe penetrates through the reaction kettle body to be connected with an external high-pressure water storage tank, and the other end of the water guide pipe is rotatably attached in the rotating groove; the top end of the cavity rotating column is communicated with the rotating groove in a flush manner; when the alcoholysis-free water spraying device works, when hydrogen chloride gas is generated in raw materials after alcoholysis, the control unit plays a role of a driving motor, the driving motor drives a rotating screw rod to rotate, the rotating screw rod rotates to drive a rotating disc to rotate in a material discharging box, meanwhile, water solution in a high-pressure water storage box can enter a water guide pipe, the bottom of the water guide pipe is attached to a rotating groove, the rotating groove is communicated with a cavity rotating column in parallel and level mode, high-pressure liquid in the water guide pipe can enter the cavity rotating column through the rotating groove, the cavity rotating column is communicated with a water spraying pipe, the high-pressure liquid in the cavity rotating column can enter the water spraying pipe, the rotating disc rotates to drive the water spraying pipe to rotate or swing in the material discharging box, the high-pressure liquid in the water spraying pipe can be sprayed into the material discharging box through water spraying holes, the sprayed liquid can absorb the hydrogen chloride gas generated in the material discharging box, and the centrifugal force of the water spraying pipe and the sprayed liquid can be increased The speed of the spray liquid is increased, and the absorption efficiency of the spray liquid to the hydrogen chloride gas is increased.
Preferably, the water guide pipe comprises a fixed pipe and a telescopic pipe; the telescopic pipe slides in the fixed pipe in a sealing way; the fixed pipe is provided with a pneumatic guide push rod, and the telescopic end of the pneumatic guide push rod is connected to the telescopic pipe through a fixed disc; a plurality of through holes are formed in the rotating disc and are positioned in the rotating groove, and the through holes are formed along the central line direction of the rotating disc; the diameter of the through hole is larger than that of the telescopic pipe, and elastic rubber sealing blocks are symmetrically arranged inside the top end of the through hole; when the deacidification device works, after deacidification is finished, the control unit controls the driving motor to slow down, an operator can enable a through hole formed in the rotating disc to be aligned with the bottom end of the telescopic pipe through the high-definition camera, after the through hole is aligned with the bottom end of the telescopic pipe, the controller of the control unit controls the pneumatic guide push rod to extend out, the pneumatic guide push rod extends out to drive the telescopic pipe to extend into the through hole through the fixed disc, and the telescopic pipe can play a role in limiting rotation on the rotating disc along with continuous extension of the telescopic pipe; an operator can put the neutralized methanol cosolvent or ammonia water into the raw materials of the discharge box through the water guide pipe, the controller controls the driving motor to rotate at the same time, the driving motor drives the rotating screw rod to rotate, the rotating disc is rotatably connected to the rotating screw rod through the ball nut pair, and the telescopic pipe plays a role in limiting rotation on the rotating disc, so that the rotating disc drives the liquid guide pipe to stir in the mixed raw materials, the neutralization effect of a neutralization product added in the raw materials is further improved, and the separation of sulfate ester in the raw materials and the equilibrium reaction rate of the raw materials are further improved; meanwhile, the filtering net film can filter high-boiling silicone oil; when the telescopic pipe does not extend into the through hole, the pipe orifice of the telescopic pipe can be tightly attached to the bottom of the rotating groove by the thrust of the pneumatic guide push rod, and the rotating disc is prevented from rotating. The high-pressure liquid is sprayed out from the orifice of the telescopic pipe.
preferably, sliding rapping blocks are arranged in a plurality of the water spray pipes in a sliding manner, and the sliding rapping blocks are arranged adjacently; the outer wall of the sliding vibrating block is sleeved with a limiting spring, one end of the limiting spring is connected with the side wall of the sliding vibrating block, and the other end of the limiting spring is connected with the inner wall of the end part of the water spraying pipe; the end part of the sliding vibration block is provided with a rubber layer, and the sliding vibration block rotates and is in extrusion contact with the inner wall of the material discharge box; when the device works, when layered high-boiling silicone oil and product water need to be filtered, the pneumatic guide push rod enables the telescopic pipe to be contracted into the rotating groove, the rotating disc drives the water spray pipe to rotate and swing at a high speed at the top end of the discharging box, the arranged sliding vibration block slides out of the water guide pipe under the action of high-speed centrifugal force, the rubber layer at the end part of the sliding vibration block can generate vibration extrusion with the inner wall of the discharging box, the vibration extrusion of the sliding vibration block and the discharging box can enable the discharging box to swing in the reaction kettle body, and the filtering and clearing of the product water and sulfate sundries can be further improved under the matching of the swinging of the discharging box and the upward movement of the sealing disk driven by the electric telescopic rod; meanwhile, the vibration of the discharging box by the sliding vibration block can prevent the phenomenon that viscous high-boiling silicone oil is bonded on the filter screen plate, and further play a role in shaking and removing the filter screen plate.
the invention has the following beneficial effects:
1. According to the invention, the spraying device is arranged to absorb hydrogen chloride gas generated after alcoholysis in the reaction kettle through the sprayed aqueous solution, and simultaneously, 30 wt% of ammonia water added in the aqueous solution can be evaporated in a high-temperature environment of the reaction kettle to generate ammonia gas, the ammonia gas and the ammonia water solution can react with the hydrogen chloride gas, and meanwhile, the evaporated ammonia water with the weight percentage lower than 30 wt% can be used for neutralizing the hydrochloric acid, so that the addition amount of the ammonia water during neutralization is reduced, and the neutralization speed of the high-boiling silicone oil is increased.
2. The rotating disc is rotatably connected to the rotating lead screw through the ball nut pair through the matching of the arranged spraying devices, the telescopic pipe plays a role in limiting rotation on the rotating disc, and the rotating disc drives the liquid guide pipe to stir in the mixed raw materials, so that the neutralization effect of a neutralization product added in the raw materials is increased, and the separation of sulfate in the raw materials and the equilibrium reaction rate of the raw materials are increased; meanwhile, the filtering net film can filter high-boiling silicone oil.
drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a flow chart of a method of the present invention;
FIG. 2 is a sectional view of a reaction vessel body of the present invention;
FIG. 3 is an assembly view of the spray assembly of the present invention;
FIG. 4 is a view of the connection of the rotating disk and the spout of the present invention;
in the figure: the device comprises a reaction kettle body 1, a discharge box 2, a sealing disc 21, a filter screen plate 22, a spraying device 3, a driving motor 31, a rotating screw rod 32, a rotating disc 33, a rotating groove 331, a concave groove 332, a through hole 333, a water guide pipe 34, a fixed pipe 35, an extension pipe 36, a cavity rotating column 37, a water spray pipe 38, a water spray hole 381, a filter screen film 382, an elastic rubber sealing block 39, a rubber swinging column 4, a rubber soft column 5, an electric telescopic rod 6, a pneumatic guide push rod 7, a fixed disc 8, a sliding vibration block 9 and a limiting spring 10.
Detailed Description
a method for producing a silicone oil according to an embodiment of the present invention will be described below with reference to fig. 1 to 4.
As shown in fig. 1 to 4, the preparation method of silicone oil of the present invention comprises the following steps:
s1: the raw material ratio is as follows: 100 parts by weight of organosilicon high-boiling residues; 30-40 parts by weight of 80-90% by weight of raw material methanol; 15-18 parts of methanol cosolvent and equal amount of urea; 1.0-1.5 parts of 27% ammonia water by weight;
s2: alcoholysis: adding 100 parts by weight of organic silicon high-boiling residues into the reaction kettle body 1 through a feeding pipe at the temperature of 20-25 ℃, dropwise adding 30-40 parts by weight of raw material methanol with the weight percentage of 80-90% for 6-8 hours; the initial dropping speed is 3 parts/hour, and the dropping time is 2-3 hours; gradually extracting to 10 parts/hour;
s3: neutralizing: adding 15-18 parts of methanol cosolvent and equal amount of urea into the materials at normal temperature, wherein the neutralization temperature is 42-50 ℃, and the neutralization time is 0.5 hour, so as to neutralize hydrochloric acid in the materials; layering to obtain crude high-boiling-point silicone oil with the pH value of 4-5, adding 0.7-1.0 part of 27% ammonia water by weight, and continuously neutralizing to ensure that the pH value is 6-8;
S4: and (3) filtering: and (3) filtering the crude high-boiling silicon oil obtained by neutralization and delamination in the step S3 through a discharge box 2 arranged in the reaction kettle body 1, and discharging filtered acid water and impurities through a discharge pipe.
As shown in fig. 1 and 2, the step S3 further includes deacidifying; deacidifying: the temperature of the reaction kettle body 1 rises to 45-60 ℃; a spray device 3 arranged in the reaction kettle body 1 is used for spraying water to absorb hydrogen chloride gas generated in the alcoholysis process; 0.2-0.5 part of 30% ammonia water in percentage by weight is mixed in the water solution of the spraying device 3; the setting through spray set 3 can absorb the aqueous solution that sprays through the hydrogen chloride gas that produces in the reaction kettle body 1 after the alcoholysis, 30% weight percent's of the aqueous ammonia that adds in the aqueous solution can evaporate the production ammonia in the environment of reaction kettle body 1 high temperature simultaneously, ammonia and aqueous ammonia solution can react with hydrogen chloride gas, the aqueous ammonia that the evaporation is less than 30% weight percent simultaneously can carry out neutralization reaction with hydrochloric acid, and then the addition of aqueous ammonia when having reduced the neutralization, accelerate the neutralization speed of high boiling silicone oil simultaneously.
As shown in fig. 2-4, a material discharging box 2 is installed in the reverse kettle body in a swinging mode through a rubber swinging column 4, the upper end of the bottom end of the material discharging box 2 is set to be in an open state, and a sealing disc 21 is arranged at the bottom end of the material discharging box 2 in a sliding mode; the sealing disc 21 is connected with the telescopic end of the electric telescopic rod 6 through the rubber soft column 5, and the bottom end of the electric telescopic rod 6 is fixed at the bottom end of the reaction kettle body 1; a plurality of filter screen plates 22 are arranged on the side wall of the upper end of the discharging box 2, and the thickness of each filter screen plate 22 is larger than that of the discharging box 2; when in work, the raw materials are put into the discharging box 2 through the charging pipe, the crude high-boiling silicone oil is obtained through the steps of alcoholysis, acid washing and neutralization, after the crude high-boiling silicone oil and the neutral product water and the sulfate are layered, the control unit controls the electric telescopic rod 6 to extend out, the electric telescopic rod 6 drives the sealing disc 21 to slide upwards in the discharging box 2, so that the silicone oil and the product water are pushed upwards after the silicon oil and the product water are layered in the discharging box 2, after the neutralized product water and sulfate move upwards to the position of the filter screen plate 22, the filter screen plate 22 will generate water and sulfate to be filtered and discharged out of the discharging box 2 along with the continuous upward movement of the sealing disc 21, the product water and sulfate discharged from the discharging box 2 will be discharged through the discharging pipe arranged at the bottom end of the reaction kettle body 1, after the product water and the sulfate are cleaned, an operator cleans the bottom end of the reaction kettle body 1 and a discharge pipe; simultaneously, the silicon oil after filtering can drive the sealing disc 21 to move downwards through the electric telescopic rod 6, the sealing disc 21 can be opened from the bottom end of the discharging box 2, and then the high-boiling silicon oil is discharged from a discharging port at the bottom end of the reaction kettle body 1.
as shown in fig. 2-4, the spraying device 3 includes a driving motor 31, a rotary screw 32, a rotary disc 33, a water conduit 34, a cavity rotary column 37 and a water spraying pipe 38; the driving motor 31 is installed at the top end of the reaction kettle body 1, and the output end of the driving motor 31 penetrates through the reaction kettle body 1 and is connected with the rotating screw rod 32; the rotating screw 32 is rotatably connected with a rotating disc 33 through a ball nut pair, and the upper surface of the rotating disc 33 is provided with a rotating groove 331; a concave groove 332 is formed in the side surface of the rotating disc 33, and a plurality of spray pipes 38 are arranged in the concave groove 332 through the cavity rotating column 37 in a swinging mode; two side walls of the water spraying pipe 38 are provided with water spraying holes 381, and the end parts of the water spraying holes 381 are provided with filter net films 382; the water spray pipe 38 is communicated with the cavity rotating column 37; one end of the water guide pipe 34 penetrates through the reaction kettle body 1 to be connected with an external high-pressure water storage tank, and the other end of the water guide pipe 34 is rotatably attached in the rotating groove 331; the top end of the cavity rotating column 37 is communicated with the rotating groove 331 in a flush manner; when the device works, when the raw materials generate hydrogen chloride gas after alcoholysis, the control unit acts as a driving motor 31, the driving motor 31 drives a rotating screw rod 32 to rotate, the rotating screw rod 32 rotates to drive a rotating disc 33 to rotate in the emptying box 2, meanwhile, water solution in a high-pressure water storage tank enters a water guide pipe 34, the bottom of the water guide pipe 34 is attached to a rotating groove 331, the rotating groove 331 is communicated with a cavity rotating column 37 in a flush manner, high-pressure liquid in the water guide pipe 34 enters the cavity rotating column 37 through the rotating groove 331, the cavity rotating column 37 is communicated with a water spray pipe 38, the high-pressure liquid entering the cavity rotating column 37 enters the water spray pipe 38, the rotating disc 33 rotates to drive the water spray pipe 38 to rotate or swing in the emptying box 2, and then the high-pressure liquid in the water spray pipe 38 is sprayed into the emptying box 2 through water spray holes 381, and the sprayed liquid can absorb the hydrogen chloride gas generated in the emptying box 2, meanwhile, the centrifugal force of the water spray pipe 38 and the rotating disc 33 which swing at a high speed can increase the area of the sprayed liquid of the water spray pipe 38 and the speed of the sprayed liquid, and further increase the absorption efficiency of the sprayed liquid on the hydrogen chloride gas.
As shown in fig. 2 to 4, the water guiding duct 34 includes a fixed duct 35 and a telescopic duct 36; the extension tube 36 slides in the fixed tube 35 in a sealing manner; the fixed tube 35 is provided with a pneumatic guide push rod 7, and the telescopic end of the pneumatic guide push rod 7 is connected to the telescopic tube 36 through a fixed disc 8; a plurality of through holes 333 are formed in the rotating disc 33, the through holes 333 are located in the rotating groove 331, and the through holes 333 are formed along the central line direction of the rotating disc 33; the diameter of the through hole 333 is larger than that of the telescopic pipe 36, and the elastic rubber sealing blocks 39 are symmetrically arranged inside the top end of the through hole 333; during operation, after deacidification is completed, the control unit controls the driving motor 31 to slow down, an operator can align the through hole 333 formed in the rotating disc 33 with the bottom end of the telescopic pipe 36 through the high-definition camera, after the through hole 333 is aligned with the bottom end of the telescopic pipe 36, the controller of the control unit controls the pneumatic guide push rod 7 to extend out, the pneumatic guide push rod 7 extends out to drive the telescopic pipe 36 to extend into the through hole 333 through the fixed disc 8, and the telescopic pipe 36 can perform limiting rotation on the rotating disc 33 along with continuous extension of the telescopic pipe 36; an operator can put the neutralized methanol cosolvent or ammonia water into the raw materials of the discharging box 2 through the water guide pipe 34, the controller controls the driving motor 31 to rotate, the driving motor 31 drives the rotating screw rod 32 to rotate, the rotating disc 33 is connected to the rotating screw rod 32 in a rotating mode through the ball nut pair, the telescopic pipe 36 plays a role in limiting rotation of the rotating disc 33, the rotating disc 33 drives the liquid guide pipe to stir in the mixed raw materials, the neutralization effect of a neutralization product added in the raw materials is increased, and then the separation of sulfate ester in the raw materials and the equilibrium reaction rate of the raw materials are increased; meanwhile, the filter net film 382 can filter high-boiling silicone oil; when the extension tube 36 is not inserted into the through hole 333, the nozzle of the extension tube 36 is tightly attached to the bottom of the rotation groove 331 by the pushing force of the pneumatic guide push rod 7, thereby preventing the rotation of the rotary disk 33. A phenomenon in which high-pressure liquid is ejected from the orifice of the bellows 36.
As shown in fig. 2-4, a plurality of sliding vibrating blocks 9 are slidably disposed in several of the spray pipes 38, and the sliding vibrating blocks 9 are disposed adjacently; the outer wall of the sliding vibrating block 9 is sleeved with a limiting spring 10, one end of the limiting spring 10 is connected with the side wall of the sliding vibrating block 9, and the other end of the limiting spring 10 is connected with the inner wall of the end part of the water spraying pipe 38; a rubber layer is arranged at the end part of the sliding vibration block 9, and the sliding vibration block 9 is in rotating extrusion contact with the inner wall of the discharging box 2; when the device works, when layered high-boiling silicone oil and product water need to be filtered, the pneumatic guide push rod 7 contracts the extension tube 36 into the rotating groove 331, the rotating disc 33 drives the water spray tube 38 to rotate and swing at a high speed at the top end of the discharging box 2, the arranged sliding vibration block slides out of the water guide tube 34 under the action of high-speed centrifugal force, the rubber layer at the end part of the sliding vibration block 9 can generate vibration extrusion with the inner wall of the discharging box 2, the vibration extrusion of the sliding vibration block 9 and the discharging box 2 can lead the discharging box 2 to swing in the reaction kettle body 1, and the vibration of the discharging box 2 and the matching of the electric telescopic rod 6 driving the sealing disc 21 to move upwards can further improve the filtering and cleaning of the product water and sulfate sundries; meanwhile, the vibration of the discharging box 2 by the sliding vibration block 9 can prevent the phenomenon that viscous high-boiling silicone oil is bonded on the filter screen plate 22, and further play a role in shaking and removing the filter screen plate 22.
The specific working process is as follows:
the raw materials are put into the discharging box 2 through the feeding pipe, after alcoholysis, the control unit plays a role of driving the motor 31, the driving motor 31 drives the rotating screw rod 32 to rotate, the rotating screw rod 32 rotates to drive the rotating disc 33 to rotate in the discharging box 2, meanwhile, the water solution in the high-pressure water storage tank enters the water guide pipe 34, the high-pressure liquid in the water guide pipe 34 enters the cavity rotating column 37 through the rotating groove 331, the rotating disc 33 rotates to drive the water spray pipe 38 to rotate or swing in the discharging box 2, further, the high-pressure liquid in the water spray pipe 38 is sprayed into the discharging box 2 through the water spray holes 381, the sprayed liquid can absorb the hydrogen chloride gas generated in the discharging box 2, after layering of crude high-boiling silicone oil and neutral product water and sulfuric ester is completed, the control unit controls the electric telescopic rod 6 to stretch out, the electric telescopic rod 6 drives the sealing disc 21 to slide upwards in the discharging box 2, after the silicone oil and the product water are layered in the discharging box 2, the silicone oil and the product water are pushed upwards, the neutralized product water and the sulfate are moved upwards to the position of the filter screen plate 22, the filter screen plate 22 can filter the produced water and the sulfate and discharge the produced water and the sulfate out of the discharging box 2 along with the continuous upward movement of the seal disc 21, the product water and the sulfate discharged from the discharging box 2 can be discharged through a discharging pipe arranged at the bottom end of the reaction kettle body 1, and after the cleaning of the product water and the sulfate is finished, an operator cleans the bottom end and the discharging pipe of the reaction kettle body 1; simultaneously, the silicon oil after filtering can drive the sealing disc 21 to move downwards through the electric telescopic rod 6, the sealing disc 21 can be opened from the bottom end of the discharging box 2, and then the high-boiling silicon oil is discharged from a discharging port at the bottom end of the reaction kettle body 1.
in the description of the present invention, it is to be understood that the terms "center", "front", "rear", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be taken as limiting the scope of the present invention.
while the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (6)
1. A preparation method of silicone oil is characterized in that: the method comprises the following steps:
S1: the raw material ratio is as follows: 100 parts by weight of organosilicon high-boiling residues; 30-40 parts by weight of 80-90% by weight of raw material methanol; 15-18 parts of methanol cosolvent and equal amount of urea; 1.0-1.5 parts of 27% ammonia water by weight;
S2: alcoholysis: adding 100 parts by weight of organic silicon high-boiling residues into a reaction kettle body (1) through a feeding pipe at the temperature of between 20 and 25 ℃, dropwise adding 30 to 40 parts by weight of raw material methanol with the weight percentage of between 80 and 90 percent, and dropwise adding for 6 to 8 hours; the initial dropping speed is 3 parts/hour, and the dropping time is 2-3 hours; gradually extracting to 10 parts/hour;
s3: neutralizing: adding 15-18 parts of methanol cosolvent and equal amount of urea into the materials at normal temperature, wherein the neutralization temperature is 42-50 ℃, and the neutralization time is 0.5 hour, so as to neutralize hydrochloric acid in the materials; layering to obtain crude high-boiling-point silicone oil with the pH value of 4-5, adding 0.7-1.0 part of 27% ammonia water by weight, and continuously neutralizing to ensure that the pH value is 6-8;
s4: and (3) filtering: and (3) filtering the crude high-boiling silicon oil obtained by neutralization and delamination in the step S3 through a discharge box (2) arranged in the reaction kettle body (1), and discharging filtered acid water and impurities through a discharge pipe.
2. The method for preparing a silicone oil according to claim 1, characterized in that: wherein the step of S3 further comprises deacidifying; deacidifying: the temperature of the reaction kettle body (1) rises to 45-60 ℃; a spraying device (3) arranged in the reaction kettle body (1) is used for spraying water to absorb hydrogen chloride gas generated in the alcoholysis process; 0.2-0.5 part of 30% ammonia water by weight is mixed in the water solution of the spraying device (3).
3. The method for preparing a silicone oil according to claim 1, characterized in that: a material discharging box (2) is arranged in the reverse kettle body in a swinging mode through a rubber swinging column (4), the upper end of the bottom end of the material discharging box (2) is in an open state, and a sealing disc (21) is arranged at the bottom end of the material discharging box (2) in a sliding mode; the sealing disc (21) is connected with the telescopic end of the electric telescopic rod (6) through the rubber soft column (5), and the bottom end of the electric telescopic rod (6) is fixed at the bottom end of the reaction kettle body (1); the side wall of the upper end of the discharging box (2) is provided with a plurality of filter screen plates (22), and the thickness of each filter screen plate (22) is larger than that of the discharging box (2).
4. The method for preparing a silicone oil according to claim 2, characterized in that: the spraying device (3) comprises a driving motor (31), a rotating screw rod (32), a rotating disc (33), a water guide pipe (34), a cavity rotating column (37) and a water spraying pipe (38); the driving motor (31) is installed at the top end of the reaction kettle body (1), and the output end of the driving motor (31) penetrates through the reaction kettle body (1) to be connected with the rotating screw rod (32); the rotating screw rod (32) is rotatably connected with a rotating disc (33) through a ball nut pair, and the upper surface of the rotating disc (33) is provided with a rotating groove (331); a concave groove (332) is formed in the side face of the rotating disc (33), and a plurality of water spraying pipes (38) are arranged in the concave groove (332) in a swinging mode through a cavity rotating column (37); two side walls of the water spraying pipe (38) are provided with water spraying holes (381), and the end part of each water spraying hole (381) is provided with a filter net film (382); the water spray pipe (38) is communicated with the cavity rotating column (37); one end of the water guide pipe (34) penetrates through the reaction kettle body (1) to be connected with an external high-pressure water storage tank, and the other end of the water guide pipe (34) is rotatably attached in the rotating groove (331); the top end of the cavity rotating column (37) is communicated with the rotating groove (331) in a flush manner.
5. The method for preparing a silicone oil according to claim 4, wherein: the water guide pipe (34) comprises a fixed pipe (35) and a telescopic pipe (36); the telescopic pipe (36) slides in the fixed pipe (35) in a sealing way; the fixed pipe (35) is provided with a pneumatic guide push rod (7), and the telescopic end of the pneumatic guide push rod (7) is connected to the telescopic pipe (36) through a fixed disc (8); a plurality of through holes (333) are formed in the rotating disc (33), the through holes (333) are located in the rotating groove (331), and the through holes (333) are formed along the central line direction of the rotating disc (33); the diameter of the through hole (333) is larger than that of the telescopic pipe (36), and an elastic rubber sealing block (39) is symmetrically arranged inside the top end of the through hole (333).
6. The method for preparing a silicone oil according to claim 4, wherein: sliding vibration blocks (9) are arranged in a plurality of the water spray pipes (38) in the plurality of water spray pipes (38) in a sliding mode, and the sliding vibration blocks (9) are arranged adjacently; the outer wall of the sliding vibration block (9) is sleeved with a limiting spring (10), one end of the limiting spring (10) is connected with the side wall of the sliding vibration block (9), and the other end of the limiting spring (10) is connected with the inner wall of the end part of the water spray pipe (38); the end part of the sliding vibration block (9) is provided with a rubber layer, and the sliding vibration block (9) is in rotating extrusion contact with the inner wall of the discharging box (2).
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| CN113599905A (en) * | 2021-08-17 | 2021-11-05 | 武汉轻工大学 | Functional component of ginseng fruit is drawed and is used extraction filter equipment |
| CN114082385A (en) * | 2021-11-16 | 2022-02-25 | 舍布有沙 | High-boiling silicon oil hydrolysis production line |
| CN114470875A (en) * | 2022-03-10 | 2022-05-13 | 新疆西部合盛硅业有限公司 | Novel efficient high-boiling silicon oil phase separation system and process |
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| US6717003B2 (en) * | 2000-02-04 | 2004-04-06 | Shin-Etsu Chemical Co., Ltd. | Silicone compound, a powder surface-treated with this compound, and a makeup containing this powder |
| CN101016383A (en) * | 2007-01-24 | 2007-08-15 | 吉林市凇泰化工有限责任公司 | Method of producing high boiling point silicon oil |
| CN102516543A (en) * | 2011-12-07 | 2012-06-27 | 唐山三友硅业有限责任公司 | Production method for preparing high-boiling silicone oil by alcoholysis of organosilicon high-boiling components |
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| CN113599905A (en) * | 2021-08-17 | 2021-11-05 | 武汉轻工大学 | Functional component of ginseng fruit is drawed and is used extraction filter equipment |
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