CN101768272B - Alkyl silicone continuous production system and production method - Google Patents
Alkyl silicone continuous production system and production method Download PDFInfo
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- CN101768272B CN101768272B CN 200910243951 CN200910243951A CN101768272B CN 101768272 B CN101768272 B CN 101768272B CN 200910243951 CN200910243951 CN 200910243951 CN 200910243951 A CN200910243951 A CN 200910243951A CN 101768272 B CN101768272 B CN 101768272B
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Abstract
The invention relates to an alkyl silicone continuous production system and a production method thereof. The production system comprises a reaction still and a washer; a first reciprocating sieve plate and a second reciprocating sieve plate are respectively arranged in the reaction still and the washer and driven to reciprocate by a motor and an eccenter; a conduit is connected between the reaction still and the washer, a tap water input conduit is arranged on the top of the washer and a water outlet is arranged at the bottom of the washer; alkylsilanol solution flows into the bottom of the washer through a conduit, and a conduit is arranged between the washer and a vacuum distillation tower; the vacuum distillation tower is communicated with a product storage pot through a conduit. The production method includes that alkylchlorosilane reactant solution and hydrolysate are prepared; alkylchlorosilane is hydrolyzed under 1-25 DEG C, the hydrolyzed silanol solution is separated from a settling chamber on the top of the washer, washed in the washer and conducted to the washer bottom through a flowmeter by 0.1-1.0 cubic meters per hour; water is sent in from the washer top through the flowmeter by 0.2-5.0 cubic meters per hour; the silanol solution is washed in countercurrent until the PH value is 6.5-7 and then condensed in vacuum to become alkyl silicone.
Description
Technical field
The present invention relates to a kind of production unit and method of silicone resin, specifically refer to take alkyl chlorosilane as raw material, utilize reaction tower and washing tower to produce continuously production system and the production method of alkyl silicone.
Background technology
The method for preparing the silicon alkyl resin has two kinds, and a kind of is with hydrocarbyl alkoxy silanes (RSi (OR ')
3, R
2Si (OR ')
2Deng) produce the silicon alkyl resin through hydrolysis, polycondensation, another kind is with chloric ether silane (RSiCl)
3, R
2SiCl
2Deng) be that raw material prepares the silicon alkyl resin by hydrolysis, polycondensation.The technical process of the second production method is short, and cost is low, is extensively adopted by people.According to bibliographical information, produce the silicon alkyl resin with second method, great majority adopt and drip the chloric ether silane in reactor, are hydrolyzed, polycondensation batch production silicon alkyl resin.As: patent CN101423611A report, after methyl chlorosilane and the mixing of phenyl chlorosilane monomer, be added drop-wise in the reactor that hydrolytic reagent is housed, carry out alcoholysis and hydrolysis reaction, prepare silicone resin through processes such as neutralization, polycondensations again.This batch production method labour intensity is large, production efficiency is low, is difficult to satisfy the production requirement of silicon alkyl resin high-quality, in enormous quantities.The continuous producing apparatus that bibliographical information silicon alkyl resin is also arranged, but document directly mixes chloric ether silane in pipeline with water, and then the reactor that the enters series connection reaction that is hydrolyzed, because chloric ether silane and water speed of response are fast, mix in pipeline that reactant often to occur crosslinked, form gel, even cause production process to stop.The present invention relates to a kind of continuous process system and method for alkyl silicone, comprise reaction tower and washing tower, the alkyl chlorosilane mixture solution enters reaction tower through liquid distributor, be dispersed into the liquid pearl of micron order particle diameter, reaction tower vibrates the sieve plate in the tower by the driven by motor eccentric wheel, makes alkyl chlorosilane liquid pearl and ethanolic soln short mix, realize rapid reaction and separate, the needs of can satisfy continuously, producing fast, production cost is low, the alkyl silicone constant product quality that obtains.
Summary of the invention
The objective of the invention is for the production unit of present alkyl silicone and the defective of method, and a kind of system that can produce continuously alkyl silicone that proposes, this system have advantages of that heat transfer rate is fast, the reactant contact area is large, detersive efficiency is high and can be continuously, stably manufactured;
The present invention also provides a kind of application production unit of the present invention to carry out the quantity-produced method, the method changes in the past by dripping alkyl chlorosilane solution in water, in reactor, carry out batch production, and the defective that the production efficiency of bringing is low, labor strength is large; And change and directly water to be mixed in pipeline with alkyl chlorosilane in the past, joining again in the cascade reaction still and produce continuously, the defective of crosslinking reaction formation gel often occurs in product; The present invention utilizes reaction tower and washing tower to carry out the alkyl silicone continuous production method to have advantages of that heat transfer rate is fast, the reactant contact area is large, production efficiency is high, labor strength is low and constant product quality.
Order of the present invention is realized by following technical proposals:
The continuous production device of alkyl silicone provided by the invention comprises that a stock chest A is communicated with at the bottom of the reaction tower E tower by pipeline C one port that volume pump is installed, and a reservoir B is communicated with the cat head of described reaction tower E by the pipeline D that volume pump is installed; It is characterized in that: also comprise a liquid distributor, washing tower L and vacuum tower R; Wherein, described liquid distributor W is installed on the bottom interior wall of reaction tower E, and the another port of described pipeline C is communicated with described liquid distributor W; Wherein, described reaction tower E is that the fixed plate I of reaction tower is cooled with circulating water with chuck temperature regulating device J; And the first reciprocating vibration sieve plate H is set in described reaction tower E, described reciprocating vibration sieve plate H is comprised of at least 10 sieve plate disk V, 1 coupling shaft U, 1 motor F and 1 eccentric wheel G, wherein, 10 sieve plate disk V are centered by coupling shaft U, parallel sleeve is contained on the coupling shaft U, by the drive of motor F and eccentric wheel G, oscillating screen plate H can reciprocating; Between the pipeline C of an installation volume pump is connected at the bottom of stock chest A and the reaction tower E tower;
The second reciprocating vibration sieve plate O is set in the described washing tower L, described reciprocating vibration sieve plate O is comprised of at least 10 sieve plate disk V, 1 coupling shaft U, 1 motor M and 1 eccentric wheel N, wherein, 10 sieve plate disk V are centered by coupling shaft U, parallel sleeve is contained on the coupling shaft U, by the drive of motor M and eccentric wheel N, oscillating screen plate O can reciprocating; Be provided with the pipeline P of under meter at described washing tower L top, with the outlet that a water is set in washing tower L bottom, alkylsilanol solution enters by the pipeline K that under meter is installed at the bottom of the tower of washing tower L, and the cat head of washing tower L is connected with vacuum tower R by the pipeline that under meter is installed; Vacuum tower R is by pipeline and a product storage tank S UNICOM.
In above-mentioned technical scheme, 0.5～1.5 meter of described reaction tower E height, 30～50 centimetres of diameters.
In above-mentioned technical scheme, 0.5～2 meter of described washing tower L height, 30～50 centimetres of diameters.
In above-mentioned technical scheme, 10～50 of described sieve plate disk quantity.
In above-mentioned technical scheme, 50 millimeters of the spacings between the described sieve plate disk have hole, 1～5 millimeter of described hole diameter, a percentage of open area 30～50% on the disk on the disk.
In above-mentioned technical scheme, the hole diameter of described liquid distributor is 40～120 microns.
The production system of a kind of silicone resin provided by the invention is carried out the quantity-produced method, it is characterized in that, comprises the steps:
1) batching
At first prepare reactant solution, according to alkyl chlorosilane: organic solvent is 30: 70～40: 60 weight ratio batching; Alkyl chlorosilane is dissolved in the organic solvent, is mixed with the alkyl chlorosilane reactant solution, with and the alkyl chlorosilane reactant solution for preparing be stored among the storage tank A;
Preparation hydrolytic reagent: according to ethanol: water is 60: 40～90: 10 weight ratio batching; Ethanol is soluble in water, be mixed with hydrolytic reagent, with and the ethanolic soln of moisture 10～40% (the quality percentage compositions) that prepare be stored in storage tank B as hydrolytic reagent;
2) hydrolysis
According to the alkyl chlorosilane reactant solution: hydrolytic reagent is 16: 84～33: 67 ratio (weight ratio) batching;
By raw material tank A with step 1) solution of the alkyl chlorosilane that is mixed with sends into from the bottom of reaction tower E by the pipeline C that volume pump is installed, flow is 0.1～1.0m
3/ h; Simultaneously, by raw material tank B ethanolic soln is sent into from the top of reaction tower E by the pipeline D that volume pump is installed, flow velocity is 0.2～6.0m
3/ h; And be open at the reciprocating vibration sieve plate of installing in the reaction tower E, and the solution of described alkyl chlorosilane is mixed with ethanolic soln, reaction is hydrolyzed; Wherein, temperature of reaction is 1～25 ℃, and the reaction times is 30～120 seconds, and the product alkylsilanol solution of described alkyl chlorosilane hydrolysis is told from reaction tower E top, and the sour water that hydrolysis reaction produces is discharged from reaction tower E bottom;
3) washing
With step 2) separate the alkylsilanol solution obtain and enter from the bottom of washing tower L through pipeline K that under meter is housed, flow is 0.1～1.0m
3/ h; Washing water are added by washing tower L top, and water temperature is 30～50 ℃, and flow is 0.2～5.0m
3/ h, and be open at the second reciprocating vibration sieve plate of installing in the washing tower L, by make sieve plate O vibration at motor M band movable eccentric wheel N, carry out countercurrent washing, alkylsilanol solution is told from the top of washing tower L after the washing, the pH value of this alkylsilanol solution is 6.5～7.0, and the sour water that washing produces is from the discharge of washing tower L bottom;
4) concentrated
Will be by step 3) alkylsilanol solution after the washing sends into vacuum tower R, at first vacuum tightness-0.07～-0.1Mpa, 40～60 ℃ of temperature steam organic solvent, collect organic solvent storage tank T;
5) polycondensation
In distillation tower (R), alkylsilanol is-0.07 at the relative vacuum degree～-0.1MPa, condensation temperature is 40～70 ℃, 0.5～2 hour polycondensation time, steam the small molecules oligopolymer, with dilution with toluene, filtration, add 0.8%～2% (quality percentage composition) catalyzer dibutyl tin dilaurate, obtain the alkyl silicone product;
In above-mentioned technical scheme, described alkyl chlorosilane comprises: METHYL TRICHLORO SILANE (MeSiCl
3), dimethyldichlorosilane(DMCS) (Me
2SiCl
2), ethyl trichlorosilane (EtSiCl
3) or diethyl dichlorosilane (Et
2SiCl
2), the perhaps at least a combination among METHYL TRICHLORO SILANE and they, described more than 2 kinds the quality percentage composition of the METHYL TRICHLORO SILANE in the combination be no less than 60%, other alkyl chlorosilane mixes according to any proportioning.
In above-mentioned technical scheme, step 1) organic solvent in is: a kind of in toluene, dimethylbenzene, ethyl acetate or the butylacetate.
The invention has the beneficial effects as follows, adopt reaction tower and washing tower with the reciprocating vibration sieve plate, can make rapidly contact between the reactant, realize rapid reaction; Alkyl chlorosilane solution is dispersed into micron-sized liquid pearl through liquid distributor, enters reaction tower, can increase the contact area of alkyl chlorosilane solution and ethanolic soln, reduces the generation of alkylsilanol crosslinking reaction; The retaining plate water cooling of reaction tower in time conducts the heat that produces, and avoids the excessive polycondensation of silanol and produces gel; The present invention is under cold condition, and the reaction that is hydrolyzed in ethanolic soln has reduced the activity of alkyl chlorosilane and water reaction, can realize rapidly, continuously, stable production; Compare advantage, the synthetic stable advantage of alkyl silicone technical indicator such as have that radiating rate is fast, the reactant contact area is large, technique is simple, reliable product quality, labor strength are low with intermittent type and other continuous production method of routine.
Description of drawings
Fig. 1 is that chloric ether silane quantity-produced of the present invention system forms (technical process) schematic diagram
Fig. 2 is the reciprocating vibration sieve structure schematic diagram in the system of the present invention
Fig. 3 is the structural representation of liquid distributor in the system of the present invention
Embodiment
Embodiment 1
With reference to figure 2, make the reciprocating vibration sieve plate in the continuous process system of the present invention, the first reciprocating vibration sieve plate H of the present embodiment is identical with the second reciprocating vibration sieve plate (O) structure, can be fixed on the coupling shaft by a plurality of sieve plate disks, coupling shaft and motor and 1 eccentric wheel connect to form.The sieve plate disk is made by polytetrafluoroethylmaterial material, and its diameter is respectively less than the internal diameter of reaction tower E or washing tower L.A plurality of sieve plate disk quantity for example can be 10,20,30 or 50, have circular opening on the sieve plate disk, and wherein percentage of open area is not less than 30%, and the diameter of disk hole is not less than 1 millimeter.The first reciprocating vibration sieve plate H is fixed on the coupling shaft U by 10 sieve plate disk suits, parallel installation between described sieve plate disk and the sieve plate disk, and 50 millimeters of the spacings between the sieve plate disk, by the drive of motor F and eccentric wheel G, the reciprocating vibration sieve plate can reciprocating.The second reciprocating vibration sieve plate O is installed on the coupling shaft U by 10 sieve plate disk V, and by the drive of motor M and eccentric wheel N, oscillating screen plate O does reciprocating; This all is that those skilled in the art can be realized.
With reference to figure 1, make the continuous process system of an alkyl silicone of the present invention, this system is by reaction tower E, the compositions such as stock chest A, reservoir B, washing tower L, the pipeline D that volume pump is installed, the pipeline K that under meter is installed and vacuum tower R; Wherein, stock chest A is communicated with at the bottom of the reaction tower E tower by the pipeline C that volume pump is installed, and reservoir B is communicated with the cat head of reaction tower E by the pipeline D that volume pump is installed.
Reaction tower E is with chuck temperature regulating device J, and the popular response tower that is cooled with circulating water of the fixed plate I of reaction tower E; Bottom interior wall at this reaction tower E is installed a liquid distributor W (as shown in Figure 3), the injection port of this liquid distributor W stretches out reaction tower E bottom, be fixed together with reaction tower E inwall, pipeline C is communicated with liquid distributor W injection port at the bottom of the reaction tower E tower.Liquid distributor W buys routine, its liquid distributor W hole diameter all can between 40～120 microns on the market.
And above-mentioned the first reciprocating vibration sieve plate H (as shown in Figure 2) is set in reaction tower E; At the bottom of the solution of alkyl chlorosilane enters reaction tower E tower by stock chest A by the pipeline C that volume pump is installed, ethanolic soln enters reaction tower E cat head by stock chest B by the pipeline D that volume pump is installed, issue the reaction of unboiled water solution in sieve plate H vibration, the solution of alkyl chlorosilane hydrolyzate enters washing tower by the pipeline K that under meter is installed; Wherein, reaction tower uses the enamel material to be made into, and for example 30 centimetres of high 0.5 meter * diameters, 35 centimetres of high 1.0 meters * diameters or high 1.5 meters * diameter are 50 centimetres.One liquid distributor, washing tower (L) and vacuum tower (R); Wherein, described liquid distributor (W) is installed on the bottom interior wall of reaction tower (E), and the another port of described pipeline (C) is communicated with described liquid distributor (W);
The second reciprocating vibration sieve plate O (as shown in Figure 2) is set in the washing tower L; With tap water as bath water, enter the cat head of washing tower by the pipeline P that under meter is installed, alkylsilanol solution is entered at the bottom of the tower by the pipeline K by the installation under meter, cat head is connected with vacuum tower R by the pipeline Q that under meter is installed, and alkylsilanol solution carries out concentrating under reduced pressure and polycondensation in vacuum tower R.Be provided with the washing water input channel P of under meter at washing tower L top, with the outlet that a water is set in washing tower L bottom, the pipeline K that under meter is installed is communicated with between at the bottom of the tower of reaction tower E top and washing tower L, alkylsilanol solution enters at the bottom of the tower of washing tower L by the pipeline K that under meter is installed, the cat head of this washing tower L is also installed one with the pipeline Q of under meter, and the other end of pipeline Q is communicated with described vacuum tower R; This vacuum tower R is by pipeline and a product (alkyl silicone) storage tank S UNICOM.Wherein, adopt the conventional washing tower L of enamel material, for example height is 0.5～2 meter, and the conventional washing tower between 30～50 centimetres of the diameters is all passable.
Vacuum tower R uses the vacuum tower of this Chemical Engineering routine.
Pipeline C is the 316L stainless steel, 25 millimeters of internal diameters.Pipeline D is carbon steel material, 25 millimeters of internal diameters.Pipeline K is the 316L material, 25 millimeters of internal diameters.
With reference to the liquid distributor W in the figure 3 making continuous process system of the present invention, in the outlet that the pipeline C that volume pump is installed enters in the reaction tower E liquid distributor W is installed, the hole diameter of liquid distributor W is 40～120 microns, the alkyl chlorosilane solution that transports from the pipeline C that volume pump is installed is dispersed into 100～500 microns liquid pearl through behind the liquid distributor; Liquid distributor W is stainless steel, uses this Chemical Engineering conventional liq sparger.
Embodiment 2
1) reactant ratio (weight ratio)
Monomethyl trichlorosilane 40
Toluene 60
2) hydrolytic reagent proportioning (weight ratio)
Ethanol 90
Water 10
At first prepare reactant solution, according to monomethyl trichlorosilane:
Toluene is40: 60 weight ratio is prepared burden, and is mixed with the toluene solution of monomethyl trichlorosilane, will be stored among the storage tank A;
Preparation hydrolytic reagent: according to ethanol: water is 90: 10 weight ratio batching; Ethanol is soluble in water, be mixed with hydrolytic reagent, be stored in storage tank B;
According to the monomethyl trichlorosilane reactant solution: hydrolytic reagent is that 16: 84 weight ratio is prepared burden;
By raw material tank A with step 1) toluene solution of the monomethyl trichlorosilane that is mixed with sends into from the bottom of reaction tower E by the pipeline C that volume pump is installed, flow is 0.1m
3/ h; Simultaneously, by raw material tank B ethanolic soln is sent into from the top of reaction tower E by the pipeline D that volume pump is installed, flow velocity is 0.55m
3/ h; And be open at the reciprocating vibration sieve plate of installing in the reaction tower E, and the solution of described alkyl chlorosilane is mixed with ethanolic soln, reaction is hydrolyzed; Wherein, temperature of reaction is 1,10 or 25 ℃, and the reaction times is 30,60 or 120 seconds, and the product alkylsilanol solution of described alkyl chlorosilane hydrolysis is told from reaction tower E top, and the sour water that hydrolysis reaction produces is discharged from reaction tower E bottom;
To separate the monomethyl silanol solution obtain from reaction tower E and enter from the bottom of washing tower L through pipeline K that under meter will be housed, and be added by washing tower L top at washing water, water temperature is 30 ℃, and flow is 0.55m
3/ h, and be open at the reciprocating vibration sieve plate of installing in the washing tower L, by make sieve plate O vibration at motor M band movable eccentric wheel N, carry out countercurrent washing, alkylsilanol solution is told from the top of washing tower L after the washing, the pH value of this alkylsilanol solution is 6.5, and the sour water that washing produces is from the discharge of washing tower L bottom;
Alkylsilanol solution after the above-mentioned washing is sent into vacuum tower R, and at first at vacuum tightness-0.07Mpa, 40 ℃ of temperature steam organic solvent, collect organic solvent storage tank T; In distillation tower R, alkylsilanol is-0.07MPa that condensation temperature is 40 ℃ at the relative vacuum degree, 0.5 hour polycondensation time steamed the small molecules oligopolymer, with dilution with toluene, filtration, can implement for dilution, filterability field technique personnel, obtain alkyl silicone.
Also comprise adding 0.8% (mass percent) catalyzer dibutyl tin dilaurate, obtain the methyl silicon resin product of 80 ℃ of curing, can be used as transparent, wear-resistant paint.
Embodiment 3
1) reactant ratio (weight ratio)
Monomethyl trichlorosilane 12～34
Dimethyldichlorosilane(DMCS) 4～32
One ethyl trichlorosilane 1～23
Butylacetate 55～60
2) hydrolytic reagent proportioning (weight ratio)
Ethanol 80
Water 20
With reference to figure 2, the continuous Production Flow Chart of preparation alkyl silicone is with embodiment 2, be pressed into raw material tank A after abovementioned alkyl chlorosilane and toluene fully mixed, ethanolic soln is pressed into another raw material tank B, ethanolic soln passes through to install the pipeline D of volume pump by the cat head adding of reaction tower, the mixture of abovementioned alkyl chlorosilane solution is passed through to install the pipeline C of volume pump from the bottom adding of reaction tower, and the mass ratio of alkyl chlorosilane solution and ethanolic soln is 25: 75; Start the motor of reaction tower, drive oscillating screen plate H, 30 beats/mins of vibration number, 5 ℃ of reactions that are hydrolyzed, 60 seconds reaction times, at the bottom of tower, emit sour water, tell silanol solution from cat head, in washing tower L, wash to pH value be 7; Silanol solution is in vacuum tower,-0.07MPa, 50 ℃, steam,-0.08Mpa, 60 ℃ of lower polycondensations 1 hour, cooling, add toluene and adjust viscosity, filter, add 1.5% (mass percent) catalyzer dibutyl tin dilaurate, obtain the alkyl silicone product of self-vulcanizing, can as buildings and road and bridge bridge pier hydrophobic coating.
Embodiment 4
1) reactant ratio (mass ratio)
Monomethyl trichlorosilane 11～24
Dimethyldichlorosilane(DMCS) 4～22
Methylethyl dichlorosilane 1～13
Dimethylbenzene 65～70
2) hydrolytic reagent proportioning (mass ratio)
Ethanol 60
Water 40
Be pressed into raw material tank A after abovementioned alkyl chlorosilane and butylacetate fully mixed, the ethanolic soln of said ratio is pressed into another raw material tank B, the pipeline of ethanolic soln by volume pump is housed added by the cat head of reaction tower E, the bottom of the pipeline of abovementioned alkyl chlorosilane solution by volume pump is housed from reaction tower E added, the weight ratio of alkyl chlorosilane solution and ethanolic soln is 33: 67, start the motor of reaction tower, drive oscillating screen plate H, 40 beats/mins of vibration number, 10 ℃ of reactions that are hydrolyzed, in 120 seconds reaction times, at the bottom of tower, emit sour water, tell alkylsilanol solution from cat head, in washing tower L, wash to pH value be 7; Abovementioned alkyl silanol solution is sent into vacuum tower R by the pipeline that under meter is housed, steam toluene-0.1Mpa, 60 ℃, then-0.1Mpa, 70 ℃ of lower polycondensations 2 hours, cooling, add toluene and adjust viscosity, filtration, adding 2% (quality percentage composition) catalyzer dibutyl tin dilaurate obtains the alkyl silicone finished product of self-vulcanizing, as high temperature resistant, insulation, hydrophobic coating.
It should be noted that; above in conjunction with the embodiments technical scheme of the present invention is had been described in detail; but those skilled in the art will find apparent that; on the technical solution of the present invention basis; can carry out variations and modifications to technical scheme of the present invention, but not break away from the model that the present invention's claims required for protection are summarized.
Claims (10)
1. the continuous process system of an alkyl silicone, comprise that a stock chest (A) is communicated with at the bottom of reaction tower (E) tower by a port of first pipeline (C) of installation volume pump, one reservoir (B) is communicated with the cat head of described reaction tower (E) by the second pipe (D) that volume pump is installed, and it is characterized in that: also comprise a liquid distributor, washing tower (L) and vacuum tower (R); Wherein, described liquid distributor (W) is installed on the bottom interior wall of reaction tower (E), and the another port of described the first pipeline (C) is communicated with described liquid distributor (W); Described reaction tower (E) is with chuck temperature regulating device (J), and the retaining plate of reaction tower (I) is cooled with circulating water; And the first reciprocating vibration sieve plate (H) is set in described reaction tower (E), described the first reciprocating vibration sieve plate (H) is comprised of at least 10 sieve plate disks (V), 1 coupling shaft (U), 1 motor (F) and 1 eccentric wheel (G), wherein, at least 10 sieve plate disks (V) are centered by this coupling shaft (U), parallel sleeve is contained on this coupling shaft (U), by the drive of motor (F) and eccentric wheel (G), the first reciprocating vibration sieve plate (H) is done reciprocating; The 3rd pipeline (K) of an installation under meter is connected between reaction tower (E) and the washing tower (L);
The second reciprocating vibration sieve plate (O) is set in the described washing tower (L), described the second reciprocating vibration sieve plate (O) is comprised of at least 10 sieve plate disks (V), 1 coupling shaft (U), 1 motor (M) and 1 eccentric wheel (N), wherein, at least 10 sieve plate disks (V) are centered by this coupling shaft (U), parallel sleeve is contained on this coupling shaft (U), by the drive of motor (M) and eccentric wheel (N), the second reciprocating vibration sieve plate (O) is done reciprocating; Be provided with the washing water input channel (P) of under meter at described washing tower (L) top, with the outlet that a water is set in washing tower (L) bottom, alkylsilanol solution enters by the 3rd pipeline (K) that under meter is installed at the bottom of the tower of this washing tower (L), and the cat head of this washing tower (L) is communicated with described vacuum tower (R) by the 4th pipeline (Q) that under meter is installed; This vacuum tower (R) is communicated with a product storage tank (S) by pipeline.
2. according to the continuous process system of alkyl silicone claimed in claim 1, it is characterized in that, described reaction tower (E) is high 0.5～1.5 meter, 30～50 centimetres of diameters.
3. according to the continuous process system of alkyl silicone claimed in claim 1, it is characterized in that 0.5～2 meter of described washing tower (L) height, 30～50 centimetres of diameters.
4. according to the continuous process system of alkyl silicone claimed in claim 1, it is characterized in that, described sieve plate disk quantity is 10～50.
5. according to the continuous process system of alkyl silicone claimed in claim 1, it is characterized in that, 50 millimeters of the spacings between the described sieve plate disk have hole on the disk, and described hole diameter is 1～5 millimeter, and the percentage of open area on the disk is 30%～50%.
6. according to the continuous process system of alkyl silicone claimed in claim 1, it is characterized in that, the hole diameter of described liquid distributor (W) is 40～120 microns.
7. an application rights requires the continuous process system of 1 described alkyl silicone to carry out the quantity-produced method, it is characterized in that, comprises the steps:
1) batching
At first prepare reactant solution: according to alkyl chlorosilane: organic solvent is the mass ratio batching of 30:70～40:60; Alkyl chlorosilane is dissolved in the organic solvent, is mixed with the alkyl chlorosilane reactant solution, and the alkyl chlorosilane reactant solution for preparing is stored in the stock chest (A);
Preparation hydrolytic reagent: according to ethanol: water is the weight ratio batching of 60:40～90:10; Ethanol is soluble in water, be mixed with hydrolytic reagent; And the hydrolytic reagent for preparing is stored in reservoir (B);
2) hydrolysis
According to the alkyl chlorosilane reactant solution: hydrolytic reagent is the weight ratio batching of 16:84～33:67;
The alkyl chlorosilane reactant solution that step 1) is prepared passes through to install first pipeline (C) of volume pump from the bottom of reaction tower (E) by stock chest (A), sends into through liquid distributor, and flow is 0.1～1.0m
3/ h; Simultaneously, by reservoir (B) ethanolic soln is sent into from the top of reaction tower (E) by the second pipe (D) that volume pump is installed, flow velocity is 0.2～6.0m
3/ h; And open the first interior reciprocating vibration sieve plate of reaction tower (E), and by the sieve plate vibration solution of described alkyl chlorosilane is mixed with ethanolic soln, reaction is hydrolyzed; Wherein, hydrolysising reacting temperature is 1～25 ℃, and the reaction times is 30～120 seconds, and the product alkylsilanol solution of described alkyl chlorosilane hydrolysis is told from reaction tower (E) top, and the sour water that hydrolysis reaction produces is discharged from reaction tower (E) bottom;
3) washing
With step 2) separate the alkylsilanol solution obtain and enter through the 3rd pipeline (K) that under meter the is installed bottom from washing tower (L), flow is 0.1～1.0m
3/ h; Washing water are added by washing tower (L) top, and water temperature is 30～50 ℃, and flow is 0.2～5.0m
3/ h, and be open at the second reciprocating vibration sieve plate of installing in the washing tower (L), and carrying out countercurrent washing, alkylsilanol solution is told from the top of washing tower (L) after the washing, the pH value of this alkylsilanol solution is 6.5～7.0, and the sour water that washing produces is discharged from washing tower (L) bottom;
4) concentrated
To send into vacuum tower (R) by the alkylsilanol solution after the step 3) washing, at first vacuum tightness-0.07～-0.1MPa, 40～60 ℃ of temperature steam organic solvent, collect organic solvent storage tank (T);
5) polycondensation
In distillation tower (R), alkylsilanol is-0.07 at the relative vacuum degree～-0.1MPa, condensation temperature is 40～70 ℃, 0.5～2 hour polycondensation time, steam the small molecules oligopolymer, with dilution with toluene, filtration, obtain alkyl silicone.
8. the continuous process system of application alkyl silicone as claimed in claim 7 is carried out the quantity-produced method, it is characterized in that, be included in also that to add the quality percentage composition in the alkyl silicone that step 5) obtains be 0.8～2% catalyzer dibutyl tin dilaurate, obtain the alkyl silicone product 25 ℃～80 ℃ of curing.
9. the continuous process system of application alkyl silicone as claimed in claim 7 is carried out the quantity-produced method, it is characterized in that, described alkyl chlorosilane comprises: METHYL TRICHLORO SILANE, dimethyldichlorosilane(DMCS), ethyl trichlorosilane or diethyl dichlorosilane, perhaps METHYL TRICHLORO SILANE and at least a combination among them, described more than 2 kinds the quality percentage composition of METHYL TRICHLORO SILANE in the combination be no less than 60%, other alkyl chlorosilane mixes according to any proportioning.
10. the continuous process system of application alkyl silicone as claimed in claim 7 is carried out continuous production method, it is characterized in that, the organic solvent in the step 1) is: toluene, dimethylbenzene, ethyl acetate or butylacetate.
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| CN 200910243951 CN101768272B (en) | 2009-12-25 | 2009-12-25 | Alkyl silicone continuous production system and production method |
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| CN102382305B (en) * | 2010-09-02 | 2013-01-02 | 上海安赐机械设备有限公司 | Alkyl chlorosilane hydrolysis device and hydrolysis process thereof |
| CN103204993B (en) * | 2013-04-16 | 2015-06-10 | 江苏大学 | Preparation method of methyl silicone resin |
| CN103834011A (en) * | 2014-02-25 | 2014-06-04 | 江苏三木化工股份有限公司 | Continuous organic silicon resin hydrolytic condensation device |
| CN105801860B (en) * | 2016-04-06 | 2019-05-21 | 衢州信步化工科技有限公司 | A kind of tower continuous production technology of poly- methyltriethoxysilane |
| CN105837821B (en) * | 2016-04-06 | 2019-05-21 | 衢州信步化工科技有限公司 | A kind of poly- methyltriethoxysilane duct type continuous production method |
| EP3625285B1 (en) * | 2017-05-16 | 2020-08-12 | Wacker Chemie AG | Method for producing organopolysiloxane resins |
| CN111630018B (en) * | 2018-01-19 | 2022-07-12 | 瓦克化学股份公司 | Alkylsilicone resins as additives for hydrophobicizing fibre cements |
| CN111004269A (en) * | 2019-12-23 | 2020-04-14 | 无锡希亚诺新材料科技有限公司 | Method and device for preparing organic silicon by hydrolyzing chlorosilane |
| CN114426667B (en) * | 2022-03-16 | 2023-07-14 | 江西海多有机硅材料股份有限公司 | Continuous preparation system and process method for MQ resin with narrow molecular weight distribution |
| CN116376021A (en) * | 2023-04-28 | 2023-07-04 | 贵州正业龙腾新材料开发有限公司 | Method and production system for continuously and controllably producing silicon resin microspheres |
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| US3855368A (en) * | 1972-04-26 | 1974-12-17 | Ceskoslovenska Akademie Ved | Apparatus for bringing fluid phases into mutual contact |
| CN101423611A (en) * | 2008-12-01 | 2009-05-06 | 金小凤 | Method for preparing high temperature resistant silicone resin |
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| US3855368A (en) * | 1972-04-26 | 1974-12-17 | Ceskoslovenska Akademie Ved | Apparatus for bringing fluid phases into mutual contact |
| CN101423611A (en) * | 2008-12-01 | 2009-05-06 | 金小凤 | Method for preparing high temperature resistant silicone resin |
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