CN103739843B - Trichlorosilane silicon tetrachloride as by-product is utilized to produce the preparation technology of ethyl polysilicate - Google Patents
Trichlorosilane silicon tetrachloride as by-product is utilized to produce the preparation technology of ethyl polysilicate Download PDFInfo
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- CN103739843B CN103739843B CN201410018619.5A CN201410018619A CN103739843B CN 103739843 B CN103739843 B CN 103739843B CN 201410018619 A CN201410018619 A CN 201410018619A CN 103739843 B CN103739843 B CN 103739843B
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 title claims abstract description 62
- 239000006227 byproduct Substances 0.000 title claims abstract description 27
- 238000005516 engineering process Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- GPATXKGIPSPFHV-UHFFFAOYSA-N Cl[SiH](Cl)Cl.Cl[Si](Cl)(Cl)Cl Chemical compound Cl[SiH](Cl)Cl.Cl[Si](Cl)(Cl)Cl GPATXKGIPSPFHV-UHFFFAOYSA-N 0.000 title claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 109
- 229960004756 ethanol Drugs 0.000 claims abstract description 40
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000012043 crude product Substances 0.000 claims abstract description 21
- 238000001704 evaporation Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000006096 absorbing agent Substances 0.000 claims abstract description 15
- 239000011552 falling film Substances 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 13
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims abstract description 7
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 4
- 239000000413 hydrolysate Substances 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000003921 oil Substances 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 230000008020 evaporation Effects 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 230000008676 import Effects 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 6
- 238000006136 alcoholysis reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 230000032050 esterification Effects 0.000 claims description 5
- 238000005886 esterification reaction Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 238000006068 polycondensation reaction Methods 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 abstract description 4
- 239000005052 trichlorosilane Substances 0.000 abstract description 4
- 230000003247 decreasing effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- -1 polysiloxane Polymers 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000002815 homogeneous catalyst Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Abstract
Invention relates to a kind of preparation technology utilizing trichlorosilane silicon tetrachloride as by-product to produce ethyl polysilicate, comprise the steps: the first step, at 85 95 DEG C of temperature, in high tower esterifying kettle, 1:0.7-1 adds silicon tetrachloride and dehydrated alcohol by volume, reaction 1.5-2h, generates other by product a small amount of such as target product ethyl polysilicate crude product and hydrogen chloride gas; Hydrogenchloride byproduct is absorbed by falling-film absorber, obtains ethyl polysilicate crude product; 2nd step, ethyl polysilicate crude product removes acid and ethanol byproducts by neutralization, rectification working process, obtains temperature and is 160-180 DEG C and evaporates point; 3rd step, after a point ethyl polysilicate mixes with water by evaporating of obtaining, is hydrolyzed, obtains hydrolysate ethyl polysilicate Si-40. The silicon tetrachloride as by-product produced in production process of trichlorosilane owing to utilizing, as raw material, had both taken full advantage of resource, and had decreased the discharge of by product, also save fund, achieve many things at one stroke.
Description
Technical field
The present invention relates to the fabricating technology field of silane coupling agent, specifically, relate to a kind of preparation technology utilizing trichlorosilane silicon tetrachloride as by-product to produce ethyl polysilicate.
Background technology
Ethyl polysilicate is the important source material of preparation silicone resin material, every compound containing Si-C key is commonly referred to as silicoorganic compound, and the compound also often by oxygen, sulphur, nitrogen etc., organic radical being connected with Siliciumatom those traditionally is used as silicoorganic compound. Wherein, taking the polysiloxane that siloxane bond (-Si-O-Si-) forms as skeleton, it is the class maximum for number in silicoorganic compound, research is dark, the most most widely used, accounts for more than the 90% of total consumption. Organosilicon, owing to having had both the performance of inorganic materials and organic materials, thus has high-low temperature resistant, electric insulation, resistance to ozone, radiation hardness, difficult combustion, hates water, the excellent specific property such as corrosion-resistant, nonpoisonous and tasteless and physiological inertia. Its main function has: sealing, encapsulation, bonding, lubrication, coating, layer pressure, surfactivity, demoulding, the bubble that disappears, foaming, crosslinked, waterproof, protection against the tide, inertia filling etc., is therefore widely used in the every profession and trades such as electric, building, chemical industry, weaving, light industry, medical treatment. Along with the lasting growth of organosilicon quantity and kind, its Application Areas is constantly widened, and forms the staple product system taken the course of its own of new chemical materials circle, and many kinds are then that other chemical cannot substitute and essential. Tetraethyl silicate is a kind of silicon organic compound, and usual said tetraethyl silicate is ethyl polysilicate Si (OC2H5)4. According to SiO in product2Content, commodity tetraethyl silicate has the multiple trade mark, ethyl polysilicate SiO2Content is about 28%(and is commonly called as Si-28). Industrial Si-30, the Si-32 etc. in addition used. Ethyl polysilicate is widely used in the industry such as protective system, organosilicon, for the manufacture of chemicals-resistant coating and heat resisting coating also as the solvent preparing organosilicon. In recent years, the presoma that ethyl polysilicate is commonly used as novel material synthesis, was subject to showing great attention to of people day by day.
Main employing two kinds of methods synthesis ethyl polysilicates in current industry: a kind of is utilize silica flour and dehydrated alcohol direct reaction under the catalysis of solubility homogeneous catalyst, generate ethyl polysilicate, another kind of method utilizes silicon tetrachloride and dehydrated alcohol reaction to prepare ethyl polysilicate, and two kinds of methods respectively have relative merits. In current industry, main employing the latter prepares ethyl polysilicate, main employing batch technology and continuously a technique.
The present invention based on synthesizing in ethyl polysilicate the respective advantage of two kinds of methods in prior art and defect develops semi-successive cultivation technique, combines both advantages, overcomes respective defect just.
Summary of the invention
It is an object of the invention to adapt to reality need, it is provided that a kind of preparation technology utilizing trichlorosilane silicon tetrachloride as by-product to produce ethyl polysilicate.
In order to realize the object of the present invention, the technical solution used in the present invention is:
A kind of preparation technology utilizing trichlorosilane silicon tetrachloride as by-product to produce ethyl polysilicate, comprise the steps: the first step, silicon tetrachloride and dehydrated alcohol is added in high tower esterifying kettle, generate target product ethyl polysilicate crude product and hydrogen chloride gas by product, hydrogenchloride byproduct, after absorbing, obtains ethyl polysilicate crude product; 2nd step, ethyl polysilicate crude product removes acid and ethanol byproducts by neutralization, rectification working process, obtains temperature and is 160-180 DEG C and evaporates point; 3rd step, after by evaporating of obtaining, a point ethyl polysilicate mixes with water, it is hydrolyzed, obtain hydrolysate ethyl polysilicate Si-40, it is characterized in that: the temperature of reaction in described high tower esterifying kettle is 85 95 DEG C, silicon tetrachloride is 1:0.7-1 with the reaction volume ratio of dehydrated alcohol, and the reaction times is 1.5-2h, and described hydrogenchloride byproduct is absorbed by falling-film absorber.
Dehydrated alcohol forms alcohol vapour by ethanol evaporation tank, and alcohol vapour out enters ethanol surge tank afterwards from ethanol evaporation tank, is out introduced into high tower afterwards from ethanol surge tank and carries out alcoholysis esterification, then enters esterifying kettle, and control flow with under meter; Described high tower is connected with falling-film absorber, and described esterifying kettle is connected with holding tank; Described silicon tetrachloride is flowed out by silicon tetrachloride storage tank, controls flow by under meter and enters high tower, then enter esterifying kettle after flowing through filter.
Alcohol vapour from ethanol surge tank out after, first open dehydrated alcohol high tower intake valve, the flow control of alcohol vapour is controlled at 40 �� 5m by under meter3/ h, controls tower top temperature at 48 �� 2 DEG C; And then open silicon tetrachloride feeding end under meter, control silicon tetrachloride flow, opens esterifying kettle thermal oil and imports and exports oil valve, control oil inlet quantity, continue control tower top temperature at 50 �� 2 DEG C, still temperature to be esterified is raised to 170 DEG C and prepares discharging, after detection sampling observation is qualified, takes out negative pressure and collects in holding tank, obtain ethyl polysilicate crude product, inspecting qualified index by random samples to be set as, in ethyl polysilicate crude product, the content of ethyl polysilicate reaches 97 98%, and pH value is between 56.
Described ethanol evaporation pressure tank controls within 0.1MPa, in evaporating pot, liquid ethanol controls below the liquid level of 1/2nd, by diaphragm control valve, nitrogen input pressure in ethanol evaporation tank is controlled between 0.2-0.25MPa, open ethanol surge tank alcohol vapour intake valve, open thermal oil terminal valve, in described ethanol surge tank, thermal oil oil temperature is at 170 190 DEG C, and in tank, ethanol temperature is at 140 160 DEG C.
Described high tower is connected with the circulating water cooling system of described falling-film absorber one end, the other end of falling-film absorber is connected with hydrochloric acid tank pump, open hydrochloric acid tank pump, described falling-film absorber negative pressure is made to reach-0.03MPa, make the negative pressure state that system keeps stable, nitrogen pressure 0.2-0.25MPa in the tank of described silicon tetrachloride storage tank.
Described ethyl polysilicate crude product in and during still carries out and, adopt sodium ethylate as neutralizing agent, import rectifying still rectifying after neutralization and obtain 160-180 DEG C evaporate point, obtain pre-product ethyl polysilicate.
Ethyl polysilicate and water are mixed according to volume ratio 1:0.28 ratio, control rectifying still temperature range by controlled cooling model discharge and it is 40-60 DEG C, then in 40min, slowly add an acidic catalyst HCL aqueous solution, then stirring, precaution of hydrolysis polycondensation process heat release is assembled and is caused quick-fried boiling, and continues reaction 1.5h, after completion of the reaction, control about 120 DEG C and carry out rectifying, remove ethanol and moisture, obtain target product ethyl polysilicate Si-40.
The useful effect of the present invention is:
1. the present invention adopts gas phase alcoholysis esterification technique, and gas-contact area is big, and reaction is more abundant, and feed stock conversion can reach more than 99%;
2. the semi-successive cultivation technique that the present invention adopts, compared with traditional technology, has the handiness of batch technology simultaneously, has again the receipts rate height of continuous process, output is big, quality good, the feature such as low in the pollution of the environment;
3. the product gone out by explained hereafter of the present invention, ethyl polysilicate Si-40 is colourless transparent liquid, and it is 39%-43% that content reaches more than 99%, SiO2 content, and acidity is less than 0.01, and viscosity is 4-7mpa.s;
Simultaneously, 4. owing to utilizing the silicon tetrachloride as by-product produced in production process of trichlorosilane as raw material, both taken full advantage of resource, and decreased the discharge of by product, also save fund, achieve many things at one stroke.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of preparation technology of the present invention;
Fig. 2 is the technical indicator of the ethyl polysilicate adopting the preparation technology of the present invention to obtain.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described:
Embodiment: see Fig. 1, Fig. 2.
The present invention discloses a kind of preparation technology utilizing trichlorosilane silicon tetrachloride as by-product to produce ethyl polysilicate, comprises the steps:
The first step, at 85 95 DEG C of temperature, in high tower esterifying kettle, 1:0.7-1 adds silicon tetrachloride and dehydrated alcohol by volume, reaction 1.5-2h, generates other by product a small amount of such as target product ethyl polysilicate crude product and hydrogen chloride gas; Hydrogenchloride byproduct is absorbed by falling-film absorber, obtains ethyl polysilicate crude product;
Concrete steps are refined as:
(1) dehydrated alcohol first forms alcohol vapour by ethanol evaporation tank, described ethanol evaporation pressure tank controls within 0.1MPa, in evaporating pot, liquid ethanol controls below the liquid level of 1/2nd, is controlled between 0.2-0.25MPa by nitrogen input pressure in ethanol evaporation tank by diaphragm control valve.
(2) alcohol vapour from ethanol evaporation tank out after, opening ethanol surge tank alcohol vapour intake valve, ethanol enters ethanol surge tank, opens thermal oil terminal valve, in described ethanol surge tank, thermal oil oil temperature is at 170 190 DEG C, and in tank, ethanol temperature is at 140 160 DEG C.
(3) alcohol vapour from ethanol surge tank out after, first open dehydrated alcohol high tower intake valve and enter high tower and carry out alcoholysis esterification, the flow control of alcohol vapour is controlled at 40 �� 5m3/h by under meter, tower top temperature is controlled at 48 �� 2 DEG C;
(4) high tower is connected with the circulating water cooling system of described falling-film absorber one end, and the other end of falling-film absorber is connected with hydrochloric acid tank pump, opens hydrochloric acid tank pump, makes described falling-film absorber negative pressure reach-0.03MPa, make the negative pressure that system keeps stable
State;
(5) silicon tetrachloride storage tank transfer valve is opened, nitrogen pressure 0.2-0.25MPa in the tank of described silicon tetrachloride storage tank, and then open silicon tetrachloride feeding end under meter to high tower charging, control silicon tetrachloride flow, open esterifying kettle thermal oil and import and export oil valve, control oil inlet quantity, continue control tower top temperature at 50 �� 2 DEG C, still temperature to be esterified is raised to and is about 170 �� 5 DEG C of preparation dischargings, after detection sampling observation is qualified, taking out negative pressure collects in holding tank, obtain ethyl polysilicate crude product, inspect qualified index by random samples to be set as, in ethyl polysilicate crude product, the content of ethyl polysilicate reaches 97 98%, pH value is between 56.
2nd step, ethyl polysilicate crude product removes acid and ethanol byproducts by neutralization, rectification working process, obtains temperature and is 160-180 DEG C and evaporates point; Ethyl polysilicate crude product in and during still carries out and, adopt sodium ethylate as neutralizing agent, import rectifying still rectifying after neutralization and obtain 160-180 DEG C evaporate point, obtain pre-product ethyl polysilicate.
3rd step, after a point ethyl polysilicate mixes with water by evaporating of obtaining, is hydrolyzed, obtains hydrolysate ethyl polysilicate Si-40.
The hydrolyzing process of the 3rd step is, ethyl polysilicate and water is mixed according to volume ratio 1:0.28 ratio, by control
Cooling water flow control rectifying still temperature range is 40-60 DEG C, then slowly adding an acidic catalyst HCL aqueous solution in 40min, add-on controls within 0.05 ratio, and this 0.05 is volume ratio, it it is the ratio of the mixed solution of the HCL aqueous solution and ethyl polysilicate and water, then stirring, precaution of hydrolysis polycondensation process heat release is assembled and is caused quick-fried boiling, and continues reaction 1.5h, after completion of the reaction, control about 120 DEG C and carry out rectifying, remove ethanol and moisture, obtain target product ethyl polysilicate Si-40.
The present invention effectively make use of during trichlorosilane synthesis is produced the silicon tetrachloride as by-product produced, and have employed high tower esterification alcoholysis process, tail gas hydrogenchloride is absorbed, be sent to trichlorosilane workshop after the process such as de-analysis and carry out recycle, decrease the discharge of tail gas, and environmental protection more.
Claims (5)
1. one kind utilizes the preparation technology of trichlorosilane silicon tetrachloride as by-product production ethyl polysilicate, comprise the steps: the first step, silicon tetrachloride and dehydrated alcohol is added in high tower esterifying kettle, generate target product ethyl polysilicate crude product and hydrogen chloride gas by product, hydrogenchloride byproduct, after absorbing, obtains ethyl polysilicate crude product; 2nd step, ethyl polysilicate crude product removes acid and ethanol byproducts by neutralization, rectification working process, obtains temperature and is 160-180 DEG C and evaporates point; 3rd step, after by evaporating of obtaining, a point ethyl polysilicate mixes with water, it is hydrolyzed, obtain hydrolysate ethyl polysilicate Si-40, it is characterized in that: the temperature of reaction in described high tower esterifying kettle is 85 95 DEG C, silicon tetrachloride is 1:0.7-1 with the reaction volume ratio of dehydrated alcohol, and the reaction times is 1.5-2h, and described hydrogenchloride byproduct is absorbed by falling-film absorber; Dehydrated alcohol forms alcohol vapour by ethanol evaporation tank, and alcohol vapour out enters ethanol surge tank afterwards from ethanol evaporation tank, is out introduced into high tower afterwards from ethanol surge tank and carries out alcoholysis esterification, then enters esterifying kettle, and control flow with under meter; Described high tower is connected with falling-film absorber, and described esterifying kettle is connected with holding tank; Described silicon tetrachloride is flowed out by silicon tetrachloride storage tank, controls flow by under meter and enters high tower, then enter esterifying kettle after flowing through filter; Alcohol vapour from ethanol surge tank out after, first open dehydrated alcohol high tower intake valve, the flow control of alcohol vapour is controlled at 40 �� 5m by under meter3/ h, controls tower top temperature at 48 �� 2 DEG C; And then open silicon tetrachloride feeding end under meter, control silicon tetrachloride flow, opens esterifying kettle thermal oil and imports and exports oil valve, control oil inlet quantity, continue control tower top temperature at 50 �� 2 DEG C, still temperature to be esterified is raised to 170 DEG C and prepares discharging, after detection sampling observation is qualified, takes out negative pressure and collects in holding tank, obtain ethyl polysilicate crude product, inspecting qualified index by random samples to be set as, in ethyl polysilicate crude product, the content of ethyl polysilicate reaches 97 98%, and pH value is between 56.
2. preparation technology according to claim 1, it is characterized in that: described ethanol evaporation pressure tank controls within 0.1MPa, in evaporating pot, liquid ethanol controls below the liquid level of 1/2nd, by diaphragm control valve, nitrogen input pressure in ethanol evaporation tank is controlled between 0.2-0.25MPa, open ethanol surge tank alcohol vapour intake valve, opening thermal oil terminal valve, in described ethanol surge tank, thermal oil oil temperature is at 170 190 DEG C, and in tank, ethanol temperature is at 140 160 DEG C.
3. preparation technology according to claim 1, it is characterized in that: described high tower is connected with the circulating water cooling system of described falling-film absorber one end, the other end of falling-film absorber is connected with hydrochloric acid tank pump, open hydrochloric acid tank pump, described falling-film absorber negative pressure is made to reach-0.03MPa, make the negative pressure state that system keeps stable, nitrogen pressure 0.2-0.25MPa in the tank of described silicon tetrachloride storage tank.
4. preparation technology according to claim 1, it is characterized in that: described ethyl polysilicate crude product in and still in carry out in and, adopt sodium ethylate as neutralizing agent, import rectifying still rectifying after neutralization and obtain 160-180 DEG C evaporate point, obtain pre-product ethyl polysilicate.
5. preparation technology according to claim 1, it is characterized in that: ethyl polysilicate and water are mixed according to volume ratio 1:0.28 ratio, control rectifying still temperature range by controlled cooling model discharge and it is 40-60 DEG C, then in 40min, slowly add an acidic catalyst HCL aqueous solution, then stir, precaution of hydrolysis polycondensation process heat release is assembled and is caused quick-fried boiling, continue reaction 1.5h, after completion of the reaction, control about 120 DEG C and carry out rectifying, remove ethanol and moisture, obtain target product ethyl polysilicate Si-40.
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| CN111303198B (en) * | 2020-01-14 | 2023-08-01 | 浙江衢州硅宝化工有限公司 | Method for preparing organosilane by using organosilicon byproduct |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634028A (en) * | 2012-04-08 | 2012-08-15 | 荆州市江汉精细化工有限公司 | Method for preparing modified tetraethoxysilane by use of waste in production of 3-chloropropyltrichlorosilane |
| CN103044476A (en) * | 2011-10-13 | 2013-04-17 | 中昊晨光化工研究院 | Method for preparing ethyl orthosilicate from polysilicon byproduct silicon tetrachloride |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044476A (en) * | 2011-10-13 | 2013-04-17 | 中昊晨光化工研究院 | Method for preparing ethyl orthosilicate from polysilicon byproduct silicon tetrachloride |
| CN102634028A (en) * | 2012-04-08 | 2012-08-15 | 荆州市江汉精细化工有限公司 | Method for preparing modified tetraethoxysilane by use of waste in production of 3-chloropropyltrichlorosilane |
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