CN101768272A - Alkyl silicone continuous production system and production method - Google Patents
Alkyl silicone continuous production system and production method Download PDFInfo
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- CN101768272A CN101768272A CN 200910243951 CN200910243951A CN101768272A CN 101768272 A CN101768272 A CN 101768272A CN 200910243951 CN200910243951 CN 200910243951 CN 200910243951 A CN200910243951 A CN 200910243951A CN 101768272 A CN101768272 A CN 101768272A
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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 be meant with the alkyl chlorosilane to be raw material, utilize the production system and the production method of reaction tower and washing tower continuous production 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) prepare the silicon alkyl resin for raw material by hydrolysis, polycondensation.Second kind of production method technical process 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 big, production efficiency is low, is difficult to satisfy the production requirement of silicon alkyl resin high-quality, in enormous quantities.The continuous production equipment that bibliographical information silicon alkyl resin is also arranged, but document directly mixes chloric ether silane in pipeline with water, and then enter the reaction that is hydrolyzed of placed in-line reactor, 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, can satisfy continuous, need of rapid production, production cost is low, the alkyl silicone constant product quality that obtains.
Summary of the invention
The objective of the invention is at the production unit of present alkyl silicone and the defective of method, and a kind of system that can the continuous production alkyl silicone that proposes, this system have that heat transfer rate is fast, the reactant contact area is big, detersive efficiency is high and can be continuously, the advantage of stably manufactured;
The present invention also provides a kind of application production unit of the present invention to carry out the quantity-produced method, this 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 big; And change and directly water to be mixed in pipeline with alkyl chlorosilane in the past, joining again and carry out continuous production in the cascade reaction still, the defective of crosslinking reaction formation gel often takes place in product; The present invention utilizes reaction tower and washing tower to carry out the alkyl silicone continuous production method to have that heat transfer rate is fast, the reactant contact area is big, production efficiency is high, labor strength is low and the advantage of 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 for having chuck temperature regulating device J, and the fixed plate I of reaction tower is cooled with circulating water; And the first reciprocating vibration sieve plate H is set in described reaction tower E, described reciprocating vibration sieve plate H is made up 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 to be the center with 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 made up 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 to be the center with 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 a 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 a 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 the solution of alkyl chlorosilane that step 1) is mixed with is sent 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, make sieve plate O vibration by drive eccentric wheel N in motor M, carry out countercurrent washing, washing back alkylsilanol solution is told from the top of washing tower L, 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) concentrate
To send into vacuum tower R by the alkylsilanol solution after the step 3) washing, at first vacuum tightness-0.07～-0.1Mpa, temperature steams organic solvent for 40～60 ℃, collects 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, the organic solvent in the step 1) is: a kind of in toluene, dimethylbenzene, ethyl acetate or the butylacetate.
The invention has the beneficial effects as follows, adopt the reaction tower and the washing tower that have the reciprocating vibration sieve plate, can make contact rapidly 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 alkyl chlorosilane and water reactive activity, can realize rapidly, continuously, stable production; Compare advantage, the advantage that synthetic alkyl silicone technical indicator is stable such as have that radiating rate is fast, the reactant contact area is big, technology 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) synoptic diagram
Fig. 2 is the reciprocating vibration sieve structure synoptic 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 present embodiment is identical with 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, 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.
The popular response tower that reaction tower E is cooled with circulating water for the fixed plate I that has chuck temperature regulating device J and reaction tower E; One liquid distributor W (as shown in Figure 3) is installed on the bottom interior wall of this reaction tower E, and the injection port of this liquid distributor W stretches out reaction tower E bottom, is fixed together with reaction tower E inwall, and 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 the above-mentioned 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 unboiled water in sieve plate H vibration and separate reaction, 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, 50 centimetres of 30 centimetres of for example high 0.5 meter * diameters, 35 centimetres of high 1.0 meters * diameters or high 1.5 meters * diameters.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 the pipeline Q of a band 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 conventional vacuum tower of this chemical industry specialty.
Pipeline C is the 316L stainless steel, 25 millimeters of internal diameters.Pipeline D is a 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 a stainless steel, uses this chemical industry specialty 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 the toluene solution of monomethyl trichlorosilane that step 1) is mixed with is sent 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, make sieve plate O vibration by drive eccentric wheel N in motor M, carry out countercurrent washing, washing back alkylsilanol solution is told from the top of washing tower L, 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, temperature steams organic solvent for 40 ℃, collects 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 80 ℃ of solidified methyl silicon resin products, 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 process of preparation alkyl silicone is with embodiment 2, to be pressed into raw material tank A behind abovementioned alkyl chlorosilane and the toluene thorough mixing, ethanolic soln is pressed into another raw material tank B, ethanolic soln passes through to install the cat head adding of the pipeline D of volume pump by reaction tower, the mixture of abovementioned alkyl chlorosilane solution is passed through to install the bottom adding of the pipeline C of volume pump from 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, vibration number 30 times/minute, 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 following 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
To be pressed into raw material tank A behind abovementioned alkyl chlorosilane and the butylacetate thorough mixing, 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, vibration number 40 times/minute, 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 following 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 generalized scope of the present invention's claims required for protection.
Claims (6)
1. the continuous process system of an alkyl silicone, comprise that a stock chest (A) is communicated with at the bottom of a reaction tower (E) tower by a port of the pipeline (C) of installation volume pump, 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); Described reaction tower (E) is for having 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), the described first reciprocating vibration sieve plate (H) is made up of at least 10 sieve plate disks (V), 1 coupling shaft (U), 1 motor (F) and 1 eccentric wheel (G); Wherein, 10 sieve plate disks (V) are to be the center with coupling shaft (U), and parallel sleeve is contained on the coupling shaft (U), and by the drive of motor (F) and eccentric wheel (G), oscillating screen plate (H) is done reciprocating; The pipeline of an installation under meter (K) 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), the described second reciprocating vibration sieve plate (O) is made up of at least 10 sieve plate disks (V), 1 coupling shaft (U), 1 motor (M) and 1 eccentric wheel (N), wherein, 10 sieve plate disks (V) are to be the center with 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) 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 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 pipeline (Q) that under meter is installed; This vacuum tower (R) is communicated with a product storage tank (S) by pipeline.
2, the continuous process system according to the described alkyl silicone of claim 1 is characterized in that, described reaction tower (E) is high 0.5～1.5 meter, 30～50 centimetres of diameters.
3, the continuous process system according to the described alkyl silicone of claim 1 is characterized in that, 0.5～2 meter of described washing tower (L) height, 30～50 centimetres of diameters.
4, the continuous process system according to the described alkyl silicone of claim 1 is characterized in that, 10～50 of described sieve plate disk quantity.
5, the continuous process system according to the described alkyl silicone of claim 1 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 the described alkyl silicone of 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 30: 70～40: 60 a mass ratio batching; 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 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 prepare be stored in storage tank (B);
2) hydrolysis
According to the alkyl chlorosilane reactant solution: hydrolytic reagent is 16: 84～33: 67 a weight ratio batching;
With step 1) be mixed with the alkyl chlorosilane reactant solution by the pipeline (C) of raw material tank (A) by under meter is installed from answering the bottom of tower (E), send into through liquid distributor, 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 under meter 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 pipeline (K) that under meter 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, washing back alkylsilanol solution is told from the top of washing tower (L), 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) concentrate
To send into vacuum tower (R) by the alkylsilanol solution after the step 3) washing, at first vacuum tightness-0.07～-0.1Mpa, temperature steams organic solvent for 40～60 ℃, collects organic solvent storage tank (S);
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. silicone resin quantity-produced method as claimed in claim 7, it is characterized in that, also be included in the catalyzer dibutyl tin dilaurate that adds 0.8～2% (quality percentage composition) in the alkyl silicone that step 7) obtains, obtain ℃ solidified alkyl silicone product 25 ℃ of (room temperature)～80.
9. silicone resin quantity-produced method as claimed in claim 7 is characterized in that described alkyl chlorosilane comprises: METHYL TRICHLORO SILANE, dimethyldichlorosilane(DMCS), ethyl trichlorosilane or diethyl dichlorosilane; 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.
10. silicone resin successive production method as claimed in claim 7 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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| CN 200910243951 CN101768272B (en) | 2009-12-25 | 2009-12-25 | Alkyl silicone continuous production system and production method |
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| CN102382305A (en) * | 2010-09-02 | 2012-03-21 | 上海安赐机械设备有限公司 | Alkyl chlorosilane hydrolysis device and hydrolysis process thereof |
| CN103204993A (en) * | 2013-04-16 | 2013-07-17 | 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 |
| CN105801860A (en) * | 2016-04-06 | 2016-07-27 | 衢州信步化工科技有限公司 | Tower-type continuous production technology of polymethyl triethoxy silane |
| CN105837821A (en) * | 2016-04-06 | 2016-08-10 | 衢州信步化工科技有限公司 | Pipeline type continuous production method of polymethyltriethoxysilane |
| CN110621722A (en) * | 2017-05-16 | 2019-12-27 | 瓦克化学股份公司 | Process for preparing organopolysiloxane resins |
| 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 |
| CN111630018A (en) * | 2018-01-19 | 2020-09-04 | 瓦克化学股份公司 | Alkylsilicone resins as additives for hydrophobicizing fibre cements |
| CN114426667A (en) * | 2022-03-16 | 2022-05-03 | 江西海多化工有限公司 | Continuous preparation system and process method of narrow molecular weight MQ resin |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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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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| CN102382305A (en) * | 2010-09-02 | 2012-03-21 | 上海安赐机械设备有限公司 | Alkyl chlorosilane hydrolysis device and hydrolysis process thereof |
| 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 |
| CN103204993A (en) * | 2013-04-16 | 2013-07-17 | 江苏大学 | Preparation method of methyl silicone resin |
| 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 |
| CN105837821A (en) * | 2016-04-06 | 2016-08-10 | 衢州信步化工科技有限公司 | Pipeline type continuous production method of polymethyltriethoxysilane |
| CN105801860A (en) * | 2016-04-06 | 2016-07-27 | 衢州信步化工科技有限公司 | Tower-type continuous production technology of polymethyl triethoxy silane |
| 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 |
| CN110621722A (en) * | 2017-05-16 | 2019-12-27 | 瓦克化学股份公司 | Process for preparing organopolysiloxane resins |
| JP2020519723A (en) * | 2017-05-16 | 2020-07-02 | ワッカー ケミー アクチエンゲゼルシャフトＷａｃｋｅｒ Ｃｈｅｍｉｅ ＡＧ | Method for producing organopolysiloxane resin |
| CN110621722B (en) * | 2017-05-16 | 2021-12-31 | 瓦克化学股份公司 | Process for preparing organopolysiloxane resins |
| CN111630018A (en) * | 2018-01-19 | 2020-09-04 | 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 |
| CN114426667A (en) * | 2022-03-16 | 2022-05-03 | 江西海多化工有限公司 | Continuous preparation system and process method of narrow molecular weight MQ resin |
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