CN102604098B - Continuous esterification production process of polyethyl silicate - Google Patents
Continuous esterification production process of polyethyl silicate Download PDFInfo
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- CN102604098B CN102604098B CN 201210042447 CN201210042447A CN102604098B CN 102604098 B CN102604098 B CN 102604098B CN 201210042447 CN201210042447 CN 201210042447 CN 201210042447 A CN201210042447 A CN 201210042447A CN 102604098 B CN102604098 B CN 102604098B
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Abstract
The invention discloses a continuous esterification production process of polyethyl silicate, belongs to the technical field of silicon chemical engineering, and particularly relates to a production process of the polyethyl silicate, in particular to a production process for directly and continuously producing the polyethyl silicate by using silicon tetrachloride with lower purity. The productionprocess comprises the following steps: performing an esterification process in a synthetic tower; pumping silicon tetrachloride and 95% ethanol used as raw materials from a tower top; filling vapour and inert light components from a 1/3 position of a tower section to keep a certain kettle temperature so as to ensure full reaction in the synthetic tower; and removing hydrogen chloride gas under vacuum and continuously extracting polyethyl silicate esterifying liquid. The purity yield of the polyethyl silicate obtained by the process meets the market requirement, the production operation is simple and easy, the labour resources are saved, the process operation is continuous and stable, and therefore, the production efficiency of an enterprise is effectively improved, and production increaseand income creating are achieved.
Description
Technical field
A kind of ethyl polysilicate continuous esterification production technique belongs to silication worker technical field, is specifically related to a kind of production technique of ethyl polysilicate, especially directly ethyl polysilicate is carried out the quantity-produced production technique with the lower silicon tetrachloride of purity.
Background technology
Ethyl polysilicate is one of main raw material of the products such as preparation chemicals-resistant coating, heat resisting coating, organic silicon solvent, precision casting binding agent and electrodeless zinc rich primer.Produce at present tetraethyl silicate and mostly adopt batch production technique: pure silicon tetrachloride and ethanol are reacted in batch still, and reacted synthetic liquid carries out rectifying, then unreacted ethanol distillation is gone out and obtains tetraethyl silicate.The batch production method is long reaction time, and unstable product quality between batch owing to can not produce continuously, needs to drop into more manpower, and production cost is high.(notification number is the inventor: CN 101701070A) in the Chinese patent of application in 2009, disclosing a kind of employing utilizes silicon tetrachloride as by-product to prepare the batch production method of ethyl polysilicate, with silicon tetrachloride as by-product without purification, being directly used in tetraethyl silicate produces again, overcome and be used further to produce tetraethyl silicate after conventional art needs first silicon tetrachloride to be purified, the high yield of cost is low, produces easily the problem of secondary pollution.Obtained preferably economic benefit.But in the production application, because foregoing invention still adopts batch production technique, it is long ubiquitous reaction time therefore can not to overcome batch production, the technical problem such as unstable product quality between batch.
Summary of the invention
Technical problem to be solved by this invention is, overcome the problem of long and unstable product quality reaction time that the higher and batch production of the production cost that exists in the production of prior art ethyl polysilicate causes, a kind of continuous esterification production technique of ethyl polysilicate is provided, the continuous esterification production technique of particularly synthesizing ethyl polysilicate with the by-product silicon tetrachloride of supervening as side reaction in the production of chloropropyl coupling agent, to realize continuous production, shorten reaction time.
The technical solution used in the present invention is: the continuous esterification production technique of this ethyl polysilicate adopts the mode of the continuous output of continuous dosing, technical process is divided into material storage, continuous esterification and material extraction three parts, its technical characterictic is, comprises following processing step:
Material storage: at normal temperatures and pressures raw material silicon tetrachloride and massfraction 95% ethanol are pressed effective silicon tetrachloride: the mass ratio batching of ethanol=1: 1.1～1.2, it is for subsequent use to be stored in respectively two raw material storage tanks;
Continuous esterification: vacuum tightness is at 0.01～0.05MPa in the control synthetic tower, raw material silicon tetrachloride and 95% ethanol are constantly sprayed into from synthetic cat head to spray into speed 150Kg/h and 158～185Kg/h respectively, the material shape that sprays into becomes to disperse the small droplets of whereabouts, ceaselessly be filled with simultaneously the air-flow that water vapour and inertia light constituent form rising from tower joint 1/3rd places, bottom, the air-flow that rises and the material drop of whereabouts form adverse current, make the fully contact in gas shock of material drop, and slow down material droplets fall speed, wherein water vapour be filled with speed be ethanol spray into speed 4.5～5.5%;
The material extraction: the ethyl polysilicate that esterification generates and excessive ethanol are from the continuously extraction of synthetic tower bottom.The product of extraction namely obtains ethyl polysilicate after removing wherein ethanol component through rectifying.
The speed that sprays into of the silicon tetrachloride of raw material described in the continuous esterification is that the speed that sprays into of 150Kg/h, 95% ethanol is 158～185Kg/h, and the mass ratio of effective silicon tetrachloride and ethanol is decided during specifically according to batching.Ethanol sprays into the preferred 175Kg/h of speed; The vacuum tightness that is filled with speed and synthetic tower of inertia light constituent is inversely proportional to, and changes at any time with vacuum tightness; Water vapour be filled with speed be ethanol spray into speed 4.5～5.5%, be preferably 5%.
Water vapour described in the continuous esterification and inertia light-component gas do not participate in reaction, discharge from the synthetic tower top to pass in the synthetic tower by heating cycle.
In the continuous esterification process, the synthetic tower head temperature is 52～58 ℃, and bottom temp is 77～83 ℃.
Described raw material silicon tetrachloride is the silicon tetrachloride as by-product of supervening as side reaction in industrial silicon tetrachloride or the production of chloropropyl coupling agent, and its content of silicon tetrachloride purity is lower, and massfraction is 92%～95%.
Ethyl polysilicate continuous esterification production technique of the present invention adopts synthetic tower to finish reaction, is provided with the dispersion jetting device of silicon tetrachloride and ethanol on the synthetic tower top, can control spraying into speed and can also making material form small droplets of material.Be provided with the inlet mouth of water vapour and inertia light-component gas at synthetic Tata joint 1/3rd places.
Compared with prior art, the beneficial effect that ethyl polysilicate continuous esterification technique of the present invention has is: adopt continuous production processes, process operation steadily reduces operation sequence and working strength, reduce human cost, the constant product quality homogeneous, raw material converting silicon tetrachloride rate reaches about 98%, and polymer silicon content is greater than 28%, shortened the reaction times, average 200 tons of single still monthly output.By product during better the digestion upstream product is produced larger alleviates environmental protection pressure, the profit growth long-term to enterprise, production safety, all very large help of tool of energy-saving and emission-reduction.
Description of drawings
Fig. 1 is the process schematic representation of the continuous esterification of ethyl polysilicate of the present invention.
Wherein, 1, silicon tetrachloride storage tank 2, the first transfering material pump 3, synthetic tower 4, synthesis reactor 5, condenser 6, esterifying liquid storage tank 7, the second transfering material pump 8, ethanol storage tank 9, the aspiration that truncates receive 10, water vapour and inertia light constituent.
Fig. 1 is the most preferred embodiment of a kind of ethyl polysilicate continuous esterification of the present invention production technique, and the present invention will be further described below in conjunction with accompanying drawing:
Embodiment
Embodiment 1
As shown in Figure 1, silicon tetrachloride storage tank 1 and ethanol storage tank 8 are connected to respectively the top of synthetic tower 3 by pipeline, silicon tetrachloride storage tank 1 connecting pipeline is provided with the first transfering material pump 2, ethanol storage tank 8 connecting pipelines are provided with the second transfering material pump 7, the top of synthetic tower 3 is provided with the spout of silicon tetrachloride and ethanol raw material, and raw material constantly sprays with the small droplets form from here when synthetic.Tower joint 1/3rd places, bottom of synthetic tower 3 are provided with inlet mouth, and water vapour and inertia light constituent 10 are filled with from here and are able to form adverse current with dripping drops.The top of synthetic tower 3 has an interface to link to each other with vacuum pump, in order to obtain reacting required subnormal ambient, and continuous sucking-off hydrogenchloride component.The bottom of synthetic tower 3 directly and synthesis reactor 4 join.The ethyl polysilicate that obtains of reaction and the ethanol of complete reaction not fall into continuously extraction behind the synthesis reactor 4 in synthetic tower 3.After condenser 5 condensations, enter esterifying liquid storage tank 6.
This ethyl polysilicate continuous esterification technique is specifically:
1, by effective silicon tetrachloride and 1: 1.10 mass ratio of ethanol batching, the by-produced tetrachlorosilane of massfraction 92% is squeezed into silicon tetrachloride storage tank 1; 95% ethanol adding ethanol storage tank 8 is stand-by;
2, driving vacuum pump vacuumizes, vacuum tightness is at 0.01～0.05MPa in the control synthetic tower 3, pump into the by-produced tetrachlorosilane raw material and pump into 95% ethanol raw material according to the speed of 158Kg/h by the speed of 150Kg/h respectively from cat head, constantly be filled with water vapour and inertia light constituent 10 from tower joint 1/3rd simultaneously, the speed that is filled with of water vapour is 8.75Kg/h, and the speed that pours of rare gas element changes at any time with vacuum tightness.Keep column bottom temperature at 80 ℃, make material abundant contact reacts in synthetic tower 3, and under vacuum hydrogen chloride gas is removed, ethyl polysilicate esterifying liquid and unreacted ethanol is continuously extraction from synthesis reactor 4; The HCl water that produces during reaction absorbs by-product hydrochloric acid processed; The water vapour that is filled with and inertia light constituent 10 are reused through thermal cycling.
3, the esterifying liquid extraction changes esterifying liquid storage tank 6 over to by condenser 5 coolings.Esterifying liquid obtains ethyl polysilicate after removing the ethanol component through simple rectifying again.Reacting effective converting silicon tetrachloride rate is 98.4%, and silicone content is 28.8% in the ethyl polysilicate that obtains.
Reaction unit is with embodiment 1, and the concrete technology step is as follows:
1, by effective silicon tetrachloride and 1: 1.20 mass ratio of ethanol batching, just the by-produced tetrachlorosilane raw material of massfraction 95% is squeezed into silicon tetrachloride storage tank 1; 95% ethanol raw material adding ethanol storage tank 8 is stand-by;
2, driving vacuum pump vacuumizes, vacuum tightness is at 0.01～0.05MPa in the control synthetic tower 3, pump into the by-produced tetrachlorosilane raw material and pump into 95% ethanol raw material according to the speed of 180Kg/h by the speed of 150Kg/h respectively from cat head, be filled with water vapour and inertia light constituent 10 from tower joint 1/3rd, the speed that is filled with of water vapour is 9.9Kg/h, and the speed that pours of rare gas element changes at any time with vacuum tightness.Keep the still temperature at 83 ℃, make material abundant contact reacts in synthetic tower 3, and under vacuum hydrogen chloride gas is removed, ethyl polysilicate esterifying liquid and unreacted ethanol is continuously extraction from synthesis reactor 4; The HCl water that produces during reaction absorbs by-product hydrochloric acid processed; The water vapour that is filled with and inertia light constituent 10 are reused through thermal cycling.
3, the esterifying liquid extraction changes esterifying liquid storage tank 6 over to by condenser 5 coolings.Esterifying liquid obtains ethyl polysilicate after deviating from the ethanol component through simple rectifying again.Reacting effective converting silicon tetrachloride rate is 98.8%, and silicone content is 29.5% in the ethyl polysilicate that obtains.
Reaction unit is with embodiment 1, and the concrete technology step is as follows:
1, by effective silicon tetrachloride and 1: 1.16 mass ratio of ethanol batching, the by-produced tetrachlorosilane raw material of massfraction 92% is squeezed into silicon tetrachloride storage tank 1; 95% ethanol raw material adding ethanol storage tank 8 is stand-by;
2, driving vacuum pump vacuumizes, vacuum tightness is at 0.01～0.05MPa in the control synthetic tower 3, pump into the by-produced tetrachlorosilane raw material and pump into 95% ethanol raw material according to the speed of 168Kg/h by the speed of 150Kg/h respectively from cat head, be filled with water vapour and inertia light constituent 10 from tower joint 1/3rd, the speed that is filled with of water vapour is 7.4Kg/h, and the speed that pours of rare gas element changes at any time with vacuum tightness.Keep the still temperature at 77 ℃, make material abundant contact reacts in synthetic tower 3, and under vacuum hydrogen chloride gas is removed, ethyl polysilicate esterifying liquid and unreacted ethanol is continuously extraction from synthesis reactor 4; The HCl water that produces during reaction absorbs by-product hydrochloric acid processed; The water vapour that is filled with and inertia light constituent 10 are reused through thermal cycling.
3, the esterifying liquid extraction changes esterifying liquid storage tank 6 over to by condenser 5 coolings.Esterifying liquid obtains ethyl polysilicate after deviating from the ethanol component through simple rectifying again.Reacting effective converting silicon tetrachloride rate is 99.2%, and the silicone content that obtains ethyl polysilicate is 29.3%.
Reaction unit is with embodiment 1, and the concrete technology step is as follows:
1, by effective silicon tetrachloride and 1: 1.14 mass ratio of ethanol batching, the by-produced tetrachlorosilane raw material of massfraction 94% is squeezed into silicon tetrachloride storage tank 1; 95% ethanol adding ethanol storage tank 8 is stand-by;
2, driving vacuum pump vacuumizes, vacuum tightness is at 0.01～0.05MPa in the control synthetic tower 3, pump into the silicon tetrachloride raw material and pump into 95% ethanol raw material according to the speed of 169Kg/h by the speed of 150Kg/h respectively from cat head, be filled with water vapour and inertia light constituent 10 from tower joint 1/3rd, the speed that is filled with of water vapour is 8.6Kg/h, and the speed that pours of rare gas element changes at any time with vacuum tightness.Keep the still temperature at 80 ℃, make material abundant contact reacts in synthetic tower 3, and under vacuum hydrogen chloride gas is removed, ethyl polysilicate esterifying liquid and unreacted ethanol is continuously extraction from synthesis reactor 4; The HCl water that produces during reaction absorbs by-product hydrochloric acid processed; The water vapour that is filled with and inertia light constituent 10 are reused through thermal cycling.
3, the esterifying liquid extraction changes esterifying liquid storage tank 6 over to by condenser 5 coolings.Esterifying liquid obtains ethyl polysilicate after removing the ethanol component through simple rectifying again.Reacting effective converting silicon tetrachloride rate is 98.6%, and the silicone content that obtains ethyl polysilicate is 28.7%.
Reaction unit is with embodiment 1, and the concrete technology step is as follows:
1, by effective silicon tetrachloride and 1: 1.10 mass ratio of ethanol batching, the industrial grade silicon tetrachloride raw material of purity 97% is squeezed into silicon tetrachloride storage tank 1; 95% ethanol adding ethanol storage tank 8 is stand-by;
2, driving vacuum pump vacuumizes, vacuum tightness is at 0.01～0.05MPa in the control synthetic tower 3, pump into the industrial grade silicon tetrachloride raw material and pump into 95% ethanol raw material according to the speed of 168Kg/h by the speed of 150Kg/h respectively from cat head, be filled with water vapour and inertia light constituent 10 from tower joint 1/3rd, the speed that is filled with of water vapour is 7.5Kg/h, and the speed that pours of rare gas element changes at any time with vacuum tightness.Keep the still temperature at 80 ℃, make material abundant contact reacts in synthetic tower 3, and under vacuum hydrogen chloride gas is removed, ethyl polysilicate esterifying liquid and unreacted ethanol is continuously extraction from synthesis reactor 4; The HCl water that produces during reaction absorbs by-product hydrochloric acid processed; The water vapour that is filled with and inertia light constituent 10 are reused through thermal cycling.
3, the esterifying liquid extraction changes esterifying liquid storage tank 6 over to by condenser 5 coolings.Esterifying liquid obtains ethyl polysilicate after removing the ethanol component through simple rectifying again.Reacting effective converting silicon tetrachloride rate is 98.5%, and the silicone content that obtains ethyl polysilicate is 28.6%.
Embodiment 6
Reaction unit is with embodiment 1, and the concrete technology step is as follows:
1, by effective silicon tetrachloride and 1: 1.20 mass ratio of ethanol batching, the industrial grade silicon tetrachloride raw material of purity 97% is squeezed into silicon tetrachloride storage tank 1; 95% ethanol adding ethanol storage tank 8 is stand-by;
2, driving vacuum pump vacuumizes, vacuum tightness is at 0.01～0.05MPa in the control synthetic tower 3, pump into the industrial grade silicon tetrachloride raw material and pump into 95% ethanol raw material according to the speed of 185Kg/h by the speed of 150Kg/h respectively from cat head, be filled with water vapour and inertia light constituent 10 from tower joint 1/3rd, the speed that is filled with of water vapour is 7.5Kg/h, and the speed that pours of rare gas element changes at any time with vacuum tightness.Keep the still temperature at 80 ℃, make material abundant contact reacts in synthetic tower 3, and under vacuum hydrogen chloride gas is removed, ethyl polysilicate esterifying liquid and unreacted ethanol is continuously extraction from synthesis reactor 4; The HCl water that produces during reaction absorbs by-product hydrochloric acid processed; The water vapour that is filled with and inertia light constituent 10 are reused through thermal cycling.
3, the esterifying liquid extraction changes esterifying liquid storage tank 6 over to by condenser 5 coolings.Esterifying liquid obtains ethyl polysilicate after removing the ethanol component through simple rectifying again.Reacting effective converting silicon tetrachloride rate is 99.2%, and the silicone content that obtains ethyl polysilicate is 29.3%.
Embodiment 7
Reaction unit is with embodiment 1, and the concrete technology step is as follows:
1, by effective silicon tetrachloride and 1: 1.15 mass ratio of ethanol batching, the industrial grade silicon tetrachloride raw material of purity 97% is squeezed into silicon tetrachloride storage tank 1; 95% ethanol adding ethanol storage tank 8 is stand-by;
2, driving vacuum pump vacuumizes, vacuum tightness is at 0.01～0.05MPa in the control synthetic tower 3, pump into the industrial grade silicon tetrachloride raw material and pump into 95% ethanol raw material according to the speed of 176Kg/h by the speed of 150Kg/h respectively from cat head, be filled with water vapour and inertia light constituent 10 from tower joint 1/3rd, the speed that is filled with of water vapour is 7.5Kg/h, and the speed that pours of rare gas element changes at any time with vacuum tightness.Keep the still temperature at 80 ℃, make material abundant contact reacts in synthetic tower 3, and under vacuum hydrogen chloride gas is removed, ethyl polysilicate esterifying liquid and unreacted ethanol is continuously extraction from synthesis reactor 4; The HCl water that produces during reaction absorbs by-product hydrochloric acid processed; The water vapour that is filled with and inertia light constituent 10 are reused through thermal cycling.
3, the esterifying liquid extraction changes esterifying liquid storage tank 6 over to by condenser 5 coolings.Esterifying liquid obtains ethyl polysilicate after removing the ethanol component through simple rectifying again.Reacting effective converting silicon tetrachloride rate is 98.8%, and the silicone content that obtains ethyl polysilicate is 29.1%.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form.The industrial grade silicon tetrachloride of purity described in the embodiment 97% only is the purity of generally speaking industry and silicon tetrachloride.Just enumerate purity among the embodiment at 92% and 95% by-produced tetrachlorosilane, by-produced tetrachlorosilane purity is 92%～95%.The equivalent embodiment that any those skilled in the art may utilize the technology contents of above-mentioned announcement to be converted and change or be modified as equivalent variations.But every technical solution of the present invention content that do not break away to any simple modification, equivalent variations and remodeling that above embodiment does, still belongs to the protection domain of technical solution of the present invention according to technical spirit of the present invention.
Claims (5)
1. an ethyl polysilicate continuous esterification production technique is characterized in that, comprises following processing step:
1.1 material storage: under the normal temperature and pressure with raw material silicon tetrachloride and massfraction be 95% ethanol by the mass ratio batching of effective silicon tetrachloride: ethanol=1:1.1～1.2, it is for subsequent use to be stored in respectively two raw material storage tanks;
1.2 continuous esterification: vacuum tightness is at 0.01～0.05MPa in the control synthetic tower, raw material silicon tetrachloride and 95% ethanol are constantly sprayed into from synthetic cat head to spray into speed 150Kg/h and 158～185Kg/h respectively, the material shape that sprays into becomes to disperse the small droplets of whereabouts, simultaneously ceaselessly be filled with water vapour from tower joint 1/3rd places, bottom and the inertia light constituent forms the air-flow that rises, wherein water vapour be filled with speed be ethanol spray into speed 4.5～5.5%;
1.3 material extraction: the ethyl polysilicate that esterification generates and excess ethyl alcohol are from the continuously extraction of synthetic tower bottom;
In the described continuous esterification process of step 1.2, the synthetic tower head temperature is 52～58 ℃, and bottom temp is 77～83 ℃.
2. ethyl polysilicate continuous esterification production technique according to claim 1, it is characterized in that: the preferred rate that sprays into of described 95% ethanol of step 1.2 is 175Kg/h.
3. ethyl polysilicate continuous esterification production technique according to claim 1 is characterized in that: the speed that is filled with of the described water vapour of step 1.2 is preferably ethanol and sprays into 5% of speed.
4. according to claim 1 or 3 described ethyl polysilicate continuous esterification production technique, it is characterized in that: the described water vapour of step 1.2 and inertia light-component gas do not participate in reaction, discharge from the synthetic tower top to pass in the synthetic tower by heating cycle.
5. ethyl polysilicate continuous esterification production technique according to claim 1 is characterized in that: described raw material silicon tetrachloride is the silicon tetrachloride as by-product that produces during industrial silicon tetrachloride or chloropropyl coupling agent are produced.
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| GB998330A (en) * | 1962-08-16 | 1965-07-14 | Monsanto Chemicals | Production of organic silicates |
| EP1113036B1 (en) * | 1999-12-28 | 2005-12-21 | General Electric Company | Continuous process for producing a silicon resin |
| CN101701070B (en) * | 2009-11-06 | 2011-07-06 | 淄博市临淄齐泉工贸有限公司 | Ethyl polysilicate synthesizing process |
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