CN105111440A - Continuous environment-friendly preparation process of methyl phenyl silicone resin for high-temperature-resistant paint - Google Patents
Continuous environment-friendly preparation process of methyl phenyl silicone resin for high-temperature-resistant paint Download PDFInfo
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- CN105111440A CN105111440A CN201510614593.5A CN201510614593A CN105111440A CN 105111440 A CN105111440 A CN 105111440A CN 201510614593 A CN201510614593 A CN 201510614593A CN 105111440 A CN105111440 A CN 105111440A
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- water
- washing
- silicone resin
- polycondensation
- hydrolysis
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- 229920002050 silicone resin Polymers 0.000 title claims abstract description 38
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000003973 paint Substances 0.000 title abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 201
- 238000005406 washing Methods 0.000 claims abstract description 196
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 64
- 239000002904 solvent Substances 0.000 claims abstract description 57
- 239000002253 acid Substances 0.000 claims abstract description 46
- 239000000463 material Substances 0.000 claims abstract description 46
- 239000005046 Chlorosilane Substances 0.000 claims abstract description 14
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000000178 monomer Substances 0.000 claims abstract description 9
- 238000004806 packaging method and process Methods 0.000 claims abstract description 3
- 230000007062 hydrolysis Effects 0.000 claims description 73
- 238000006460 hydrolysis reaction Methods 0.000 claims description 73
- 238000003756 stirring Methods 0.000 claims description 54
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 44
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 31
- 239000011248 coating agent Substances 0.000 claims description 25
- 238000000576 coating method Methods 0.000 claims description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 21
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 12
- 239000011701 zinc Substances 0.000 claims description 12
- 229910052725 zinc Inorganic materials 0.000 claims description 12
- 150000001555 benzenes Chemical class 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 230000005587 bubbling Effects 0.000 claims description 7
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 claims description 7
- OSXYHAQZDCICNX-UHFFFAOYSA-N dichloro(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](Cl)(Cl)C1=CC=CC=C1 OSXYHAQZDCICNX-UHFFFAOYSA-N 0.000 claims description 7
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 7
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- UFWIBTONFRDIAS-UHFFFAOYSA-N naphthalene-acid Natural products C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 6
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 claims description 6
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 2
- 125000005609 naphthenate group Chemical group 0.000 claims description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 2
- 239000000413 hydrolysate Substances 0.000 abstract description 31
- 238000000034 method Methods 0.000 abstract description 25
- 239000000047 product Substances 0.000 abstract description 14
- 238000002156 mixing Methods 0.000 abstract description 6
- 239000002351 wastewater Substances 0.000 abstract description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract 3
- 238000007599 discharging Methods 0.000 abstract 1
- 239000011261 inert gas Substances 0.000 abstract 1
- 230000007935 neutral effect Effects 0.000 abstract 1
- 239000005416 organic matter Substances 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 238000004065 wastewater treatment Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 20
- 239000002994 raw material Substances 0.000 description 13
- 230000000694 effects Effects 0.000 description 12
- 230000003068 static effect Effects 0.000 description 11
- 238000003860 storage Methods 0.000 description 11
- 238000000746 purification Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 6
- 238000004821 distillation Methods 0.000 description 5
- 238000009776 industrial production Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000008096 xylene Substances 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- -1 siloxanes Chemical class 0.000 description 4
- 230000003301 hydrolyzing effect Effects 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 2
- CVOFKRWYWCSDMA-UHFFFAOYSA-N 2-chloro-n-(2,6-diethylphenyl)-n-(methoxymethyl)acetamide;2,6-dinitro-n,n-dipropyl-4-(trifluoromethyl)aniline Chemical compound CCC1=CC=CC(CC)=C1N(COC)C(=O)CCl.CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O CVOFKRWYWCSDMA-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003851 biochemical process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- 238000007086 side reaction Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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- Paints Or Removers (AREA)
- Silicon Polymers (AREA)
Abstract
The invention relates to a continuous environment-friendly preparation process of methyl phenyl silicone resin for high-temperature-resistant paint. The technical scheme includes: mixing according to a mass ratio of 1-20:1-10:1-10:1-20, and entering a tubular hydrolyzer to react with diluted acid water, wherein mass of benzene solvent is 1-3 times that of mixed chlorosilane monomer, and mass of the diluted acid water is 2-5 times that of the mixed chlorosilane monomer; stepwise washing hydrolysate at three or more stages to be neutral; continuously concentrating in vacuum, and allowing polycondensation when materials in a concentration polycondensation kettle reach 50-60% of volume of the kettle; after polycondensation is completed, detecting, filtering, packaging and recycling the solvent. The process has the advantages that no wastewater is discharged, the problem that conventional processes are large in discharging quantity, high in organic matter content and difficult in wastewater treatment is solved, product yield is increased, and devolatiligation time is reduced by feeding inert gas in the process of polycondensation.
Description
Technical field
The present invention relates to a kind of synthetic method of methyl phenyl silicone resin, specifically refer to a kind of continuous environment-friendly preparation process of high-temperature resistant coating methyl phenyl silicone resin.
Background technology
Because silicone resin has the characteristics such as heat-resisting, cold-resistant, moistureproof, weather-proof, therefore there is considerable status in speciality coating industry.Organosilicon coating various in style, roughly can divide into heat-resisting, weather-proof protective system, resistance to scratch Clear paint, the demoulding and moisture-proof coating and radiation resistant coating etc.High-temperature resistant coating methyl phenyl silicone resin can more than 200 DEG C life-time service, the change of film color, gloss is little and film is complete, do not have fracture phenomena.Organosilicon coating is the highest can 1400 DEG C of uses.Organosilicon coating is obtained in new product development and application aspect and develops very rapidly in recent years.
The preparation of methyl phenyl silicone resin is mainly divided into organoalkoxysilane by starting material difference and is raw material and is raw material two kinds of routes with chlorosilane.Low owing to utilizing chlorosilane monomer to produce silicone resin cost, main product is still raw material production with chlorosilane both at home and abroad at present.Mixed chlorosilane monomer is hydrolyzed under the protection of benzene series Solvents Solvent prepares methyl phenyl silicone resin; in traditional batch hydrolysis process; needing large water gaging repeatedly to wash just can make hydrolyzate wash neutrality; produce 1 ton of methyl phenyl silicone resin and about produce 10 ~ 15 tons of washess; not only contaminate environment, and can product yield be reduced.Benzene series solvent and siloxanes can be carried secretly, therefore acid waste water biodegradability extreme difference in washing diluted acid water, conventional biochemical process can not be adopted to process.Be difficult to solve just because of environmental issue, along with country and local environmental protection policy are increasingly strict, domestic many production methyl phenyl silicone resin enterprises close down.Refer to the harm of silicone resin waste water in CN101602559B, its treatment process mentioned is comparatively complicated, more difficultly realizes industrialization.CN103694477A adopts organoalkoxysilane to be that methyl phenyl silicone resin prepared by raw material, and it adopts oil in the mode separating acid of membrane sepn and rectifying, diluted acid and alcohol, and facility investment is comparatively large, and energy consumption is higher.For the state-of-the-art utilizing chlorosilane to prepare methyl phenyl silicone resin, develop a kind of environmental protection, efficient production technique work is significant to industry development.
Meanwhile, hydrolyzing chlorosilane thing also need carry out polycondensation after being washed to neutrality under catalyst action, makes the hydroxyl in hydrolyzing chlorosilane thing reduce to certain limit, and downstream client is solidified in use faster, the small molecules that solidification process is deviate from is less.Because material viscosity is comparatively large in existing technique, mass-and heat-transfer effect is poor, average 4 ~ 10 hours of polycondensation process reaction times, polycondensation reaction time is long, cause production efficiency lower, production energy consumption is large, thus develops the reaction unit being more applicable to polycondensation link significant.
Summary of the invention
The present invention is directed to deficiency of the prior art, propose a kind of methyl phenyl silicone resin preparation technology of continuous environmental protection, can non-wastewater discharge be realized, and shorten polycondensation reaction time, improve product production.
The present invention adopts following technical scheme:
A continuous environment-friendly preparation process for high-temperature resistant coating methyl phenyl silicone resin, carries out as follows:
A, hydrolysis
Phenyl-trichloro-silicane, diphenyl dichlorosilane, METHYL TRICHLORO SILANE, dimethyldichlorosilane(DMCS) 1 ~ 20:1 in mass ratio ~ 10:1 ~ 10:1 ~ 20 mix, the quality of benzene series solvent is 1 ~ 3 times of mixed chlorosilane monomer mass, after enter pipe type water solution reactor and diluted acid water reacts, the quality of diluted acid water is 2 ~ 5 times of mixed chlorosilane monomer mass, hydrolysis temperature is 10 ~ 60 DEG C, hydrolysis gauge pressure 0.3 ~ 0.5MPa, after charging completes, material is 2 ~ 30 minutes in the hydrolysis system residence time;
B, washing
Hydrolyzate is washed to neutrality step by step through more than three grades or three grades, washing temperature 30 ~ 80 DEG C, after three grades of washings, water is used as secondary washing, after secondary washing, water is used as one-level washing, after one-level washing, water enters tubular reactor as hydrolysis medium, and the water consumption that water rinses is added equals the washing water consumption entering tubular type hydrolysis reactor;
C, concentrated and polycondensation
Carry out continuous concentration at vacuum tightness 0 ~ 0.098MPa, when material reaches 50% ~ 60% of still volume in polycondensation vessel to be concentrated, add catalyzer, carry out polycondensation, temperature of reaction 120 ~ 160 DEG C, react 2 ~ 4 hours, open bubbling device bottom concentrated polycondensation vessel, blast rare gas element;
D, detection, filtration, packaging, recycled solvent
Add benzene series solvent after polycondensation completes and reach 50% mass ratio to the said products effective content mass ratio, pack after filtration, become silicone resin finished product.
Beneficial effect of the present invention:
This programme by-product mass concentration is 10 ~ 30% hydrochloric acid, non-wastewater discharge, because the solvent carried secretly in washing diluted acid water and siloxanes all return hydrolysis system, can solve in traditional technology that to wash sour water quantity discharged large, many containing organism, the unmanageable difficult problem of waste water, can improve product yield simultaneously.By the stirring of rare gas element with take effect out of in polycondensation process, improve low molecular deviate from degree, shorten the de-low time.Simultaneously due to the provide protection of rare gas element, siloxanes is lower in high-temperature polycondensation stage oxidation degree, effectively avoids Yellowing.Compared to traditional intermittent hydrolysis technical process, under normal continuous seepage condition, the stable process conditions of each unit in whole production system, in hydrolytic process, side reaction resultant output controls within the specific limits, the polysiloxane macromonomer molecular weight distribution that hydrolysis is formed is average, and product performance are more excellent.
This product can prepare the heat resisting coating of resistance to 100 ~ 700 DEG C.
Further, preferred version of the present invention:
In step a diluted acid water to be mass concentration when quantity-produced the first still be 0.9% dilute hydrochloric acid, diluted acid water selected is afterwards the washing water in a upper still water washing process after one-stage water wash.
In step a, benzene series solvent is dimethylbenzene.
Water washing process processing condition in step b: condition of normal pressure, washing kettle adopts frame type stirring, and stirring velocity 80 ~ 120 revs/min, washing time at different levels is 8 ~ 12 minutes.
Frame type stirring is adopted, stirring velocity 80 ~ 120 revs/min in step c.
Catalyzer used in step c is naphthenate or the octylate of metallic zinc, be naphthalene acid zinc, zinc octoate, isocaprylic acid zinc one of them.
In step c, the add-on of catalyzer is 0.5 ~ 5 ‰ of hydrolyzate quality.
Rare gas element described in step c is nitrogen.
When carrying out polycondensation in step c, vacuum tightness is 0 ~ 0.098MPa.
Accompanying drawing explanation
Accompanying drawing is process flow diagram of the present invention, wherein 11: static mixer; 12: tubular reactor; 13: preseparator; 14: hydrolysis recycle pump; 15: hydrolysis water cooler; 16: acid separator; 17 hydrochloric acid cleaners;
21: one-stage water wash still; 22: primary oil water separator; 23: one-stage water wash recycle pump; 24: secondary washing kettle; 25: secondary water-and-oil separator; 26: secondary water washing cycles pump; 27: tertiary effluent washes still; 28: three grades of water-and-oil separators; 29: tertiary effluent washes recycle pump;
31: hydrolyzate storage tank; 32: concentrated polycondensation vessel; 33: solvent recovery tank; 34: solvent condenser; 35: solvent delivery pump;
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1
A continuous environment-friendly preparation process for high-temperature resistant coating methyl phenyl silicone resin, carries out as follows:
According to following proportioning raw materials charging:
Phenyl-trichloro-silicane: 42kg/h; Diphenyl dichlorosilane: 8kg/h
METHYL TRICHLORO SILANE: 10kg/h; Dimethyldichlorosilane(DMCS): 17kg/h
Dimethylbenzene: 160kg/h; Diluted acid water: 240kg/h
A, hydrolysis
Chlorosilane monomer and dimethylbenzene are dosed in static mixer according to said ratio, after static mixer 11 tentatively mixing, enter pipe type water solution reactor 12, react with diluted acid water.Diluted acid water to be mass concentration be 0.9% dilute hydrochloric acid (also can adopt the washing water after one-stage water wash in a still material water washing process).Be 30 DEG C by hydrolysis water cooler 15 controlled hydrolysis temperature, reaction table pressure 0.4MPa in hydrolysis reactor, after charging completes, material is 10 minutes in the hydrolysis system residence time.Heat exchange in hydrolysis water cooler 15 is transported material to by hydrolysis recycle pump 14, then enter into preseparator 13 and carry out pre-separation, again by Pipeline transport in acid separator 16, hydrolysate flows out through acid separator 16 upper outlet, be delivered to one-stage water wash still 21 to wash, stirring velocity 100 revs/min; Acid separator 16 lower floor solution goes out to hydrochloric acid cleaner 17 through separator bottom stream, and solution, after hydrochloric acid cleaner 17 purifies, stores, can be used for other industrial production.
B, washing
Hydrolysate is washed till neutrality through tertiary effluent, and during washing, in still, mixeding liquid temperature controls at 50 DEG C, condition of normal pressure.
Water used in water washing process adopts common process water when the first still, and water is afterwards the washing water (the common process water of the hydromining that last step adds) after next stage washing.
Hydrolysate is introduced into one-stage water wash still 21 and cleans, washing kettle adopts frame type stirring, stirring velocity 100 revs/min, washing time 10 minutes, control washing water flow 240kg/h, then enter into primary oil water separator 22 and carry out oily water separation, lower floor's washing soln is driven into tubular type hydrolysis reactor 12 through one-stage water wash recycle pump 23, and the lower floor's washing soln after one-level washing enters the hydrolysis medium that tubular type hydrolysis reactor 12 reacts as next still; Upper materials component is delivered to secondary washing kettle 24.
Hydrolysate enters secondary washing kettle 24 and cleans, washing kettle adopts frame type stirring, stirring velocity 100 revs/min, washing time 10 minutes, control washing water flow 240kg/h, then enter into secondary water-and-oil separator 25 and carry out oily water separation, lower floor's washing soln is driven into one-stage water wash still 21 through secondary water washing cycles pump 26, and the washing water after secondary washing are used as one-level washing water and use; Upper materials component is delivered to tertiary effluent and washes still 27.
Hydrolysate enters tertiary effluent and washes still 27 and clean, washing kettle adopts frame type stirring, stirring velocity 100 revs/min, washing time 10 minutes, control washing water flow 240kg/h, then enter into three grades of water-and-oil separators 28 and carry out oily water separation, lower floor's washing soln through tertiary effluent wash recycle pump 29 be driven into secondary washing kettle 24, three grades washing after washing water be used as secondary washing water use; Upper materials component is delivered to hydrolyzate storage tank 31.
After washing terminates, to realize water-and-oil separator interface by interface automatic control technology constant, thus realize being separated of washing water and oily matter.
C, concentrated and polycondensation
Hydrolysate is delivered to concentrated polycondensation vessel 32 from hydrolyzate storage tank 31, continuous concentration is carried out under vacuum tightness 0 ~ 0.098MPa, deviate from solvent, solvent is delivered to solvent recovery tank 33 through solvent cooler 34, recovered solvent is delivered to distillation purification workshop section through solvent delivery pump 35, and the solvent after purification can be recycled and reused for hydrolysis system.
When material reaches 60% of still volume in polycondensation vessel 32 to be concentrated, carry out polycondensation, add naphthalene acid zinc, add that quality is hydrolyzate quality 3 ‰ of naphthalene acid zinc, polycondensation temperature is 150 DEG C, and vacuum tightness is 0.090Mpa, grid agitator stirring velocity is 100 revs/min, reacts 4 hours.
When carrying out polycondensation, open vacuum pump, open nitrogen bubble device at the bottom of concentrated polycondensation vessel 32 still, by the stirring of nitrogen with take effect out of, improve low molecular deviate from degree, shorten the de-low time, because a small amount of nitrogen intake just can play the effect of bubbling, so blast nitrogen not affect vacuum.
Add xylene solvent to above-mentioned material effective content mass ratio after polycondensation completes and reach 50%, pack after filtration, obtained silicone resin finished product.
Embodiment 2
A continuous environment-friendly preparation process for high-temperature resistant coating methyl phenyl silicone resin, carries out as follows:
According to following proportioning raw materials charging:
Phenyl-trichloro-silicane: 50kg/h; Diphenyl dichlorosilane: 6kg/h
METHYL TRICHLORO SILANE: 4kg/h; Dimethyldichlorosilane(DMCS): 17kg/h
Dimethylbenzene: 160kg/h; Diluted acid water: 320kg/h
A, hydrolysis
Raw material is dosed in static mixer according to said ratio, after static mixer 11 tentatively mixing, enters pipe type water solution reactor 12, react with diluted acid water.Diluted acid water to be mass concentration be 0.8% dilute hydrochloric acid (also can adopt the washing water after one-stage water wash in a still material water washing process).Be 20 DEG C by hydrolysis water cooler 15 controlled hydrolysis temperature, reaction table pressure 0.3MPa in hydrolysis reactor, after charging completes, material is 8 minutes in the hydrolysis system residence time.Heat exchange in hydrolysis water cooler 15 is transported material to by hydrolysis recycle pump 14, then enter into preseparator 13 and carry out pre-separation, again by Pipeline transport in acid separator 16, hydrolysate flows out through acid separator 16 upper outlet, be delivered to one-stage water wash still 21 to wash, stirring velocity 110 revs/min; Acid separator 16 lower floor solution goes out to hydrochloric acid cleaner 17 through separator bottom stream, and solution, after hydrochloric acid cleaner 17 purifies, stores, can be used for other industrial production.
B, washing
Hydrolysate is washed till neutrality through tertiary effluent, and during washing, in still, mixeding liquid temperature controls at 30 DEG C, condition of normal pressure.
Water used in water washing process adopts common process water when the first still, and water is afterwards the washing water (the common process water of the hydromining that last step adds) after next stage washing.
Hydrolysate is introduced into one-stage water wash still 21 and cleans, washing kettle adopts frame type stirring, stirring velocity 110 revs/min, washing time 11 minutes, control washing water flow 320kg/h, then enter into primary oil water separator 22 and carry out oily water separation, lower floor's washing soln is driven into tubular type hydrolysis reactor 12 through one-stage water wash recycle pump 23, and the lower floor's washing soln after one-level washing enters the hydrolysis medium that tubular type hydrolysis reactor 12 reacts as next still; Upper materials component is delivered to secondary washing kettle 24.
Hydrolysate enters secondary washing kettle 24 and cleans, washing kettle adopts frame type stirring, stirring velocity 110 revs/min, washing time 11 minutes, control washing water flow 320kg/h, then enter into secondary water-and-oil separator 25 and carry out oily water separation, lower floor's washing soln is driven into one-stage water wash still 21 through secondary water washing cycles pump 26, and the washing water after secondary washing are used as one-level washing water and use; Upper materials component is delivered to tertiary effluent and washes still 27.
Hydrolysate enters tertiary effluent and washes still 27 and clean, washing kettle adopts frame type stirring, stirring velocity 110 revs/min, washing time 11 minutes, control washing water flow 320kg/h, then enter into three grades of water-and-oil separators 28 and carry out oily water separation, lower floor's washing soln through tertiary effluent wash recycle pump 29 be driven into secondary washing kettle 24, three grades washing after washing water be used as secondary washing water use; Upper materials component is delivered to hydrolyzate storage tank 31.
After washing terminates, to realize water-and-oil separator interface by interface automatic control technology constant, thus realize being separated of washing water and oily matter.
C, concentrated and polycondensation
Hydrolysate is delivered to concentrated polycondensation vessel 32 from hydrolyzate storage tank 31, continuous concentration is carried out under vacuum tightness 0 ~ 0.098MPa, deviate from solvent, solvent is delivered to solvent recovery tank 33 through solvent cooler 34, recovered solvent is delivered to distillation purification workshop section through solvent delivery pump 35, and the solvent after purification can be recycled and reused for hydrolysis system.
When material reaches 55% of still volume in polycondensation vessel 32 to be concentrated, carry out polycondensation, add naphthalene acid zinc, add that quality is hydrolyzate quality 2 ‰ of naphthalene acid zinc, polycondensation temperature is 140 DEG C, and vacuum tightness is 0.090Mpa, grid agitator stirring velocity is 110 revs/min, reacts 3 hours.
When carrying out polycondensation, open vacuum pump, open nitrogen bubble device at the bottom of concentrated polycondensation vessel 32 still, by the stirring of nitrogen with take effect out of, improve low molecular deviate from degree, shorten the de-low time, because a small amount of nitrogen intake just can play the effect of bubbling, so blast nitrogen not affect vacuum.
Add xylene solvent to above-mentioned material effective content mass ratio after polycondensation completes and reach 50%, pack after filtration, obtained silicone resin finished product.
Embodiment 3
A continuous environment-friendly preparation process for high-temperature resistant coating methyl phenyl silicone resin, carries out as follows:
According to following proportioning raw materials charging:
Phenyl-trichloro-silicane: 57kg/h; Diphenyl dichlorosilane: 6kg/h
METHYL TRICHLORO SILANE: 4kg/h; Dimethyldichlorosilane(DMCS): 20kg/h
Dimethylbenzene: 160kg/h; Diluted acid water: 240kg/h
A, hydrolysis
Raw material is dosed in static mixer according to said ratio, after static mixer 11 tentatively mixing, enters pipe type water solution reactor 12, react with diluted acid water.Diluted acid water to be mass concentration be 0.5% dilute hydrochloric acid (also can adopt the washing water after one-stage water wash in a still material water washing process).Be 40 DEG C by hydrolysis water cooler 15 controlled hydrolysis temperature, reaction table pressure 0.5MPa in hydrolysis reactor, after charging completes, material is 15 minutes in the hydrolysis system residence time.Heat exchange in hydrolysis water cooler 15 is transported material to by hydrolysis recycle pump 14, then enter into preseparator 13 and carry out pre-separation, again by Pipeline transport in acid separator 16, hydrolysate flows out through acid separator 16 upper outlet, be delivered to one-stage water wash still 21 to wash, stirring velocity 90 revs/min; Acid separator 16 lower floor solution goes out to hydrochloric acid cleaner 17 through separator bottom stream, and solution, after hydrochloric acid cleaner 17 purifies, stores, can be used for other industrial production.
B, washing
Hydrolysate is washed till neutrality through tertiary effluent, and during washing, in still, mixeding liquid temperature controls at 40 DEG C, condition of normal pressure.
Water used in water washing process adopts common process water when the first still, and water is afterwards the washing water (the common process water of the hydromining that last step adds) after next stage washing.
Hydrolysate is introduced into one-stage water wash still 21 and cleans, washing kettle adopts frame type stirring, stirring velocity 90 revs/min, washing time 12 minutes, control washing water flow 240kg/h, then enter into primary oil water separator 22 and carry out oily water separation, lower floor's washing soln is driven into tubular type hydrolysis reactor 12 through one-stage water wash recycle pump 23, and the lower floor's washing soln after one-level washing enters the hydrolysis medium that tubular type hydrolysis reactor 12 reacts as next still; Upper materials component is delivered to secondary washing kettle 24.
Hydrolysate enters secondary washing kettle 24 and cleans, washing kettle adopts frame type stirring, stirring velocity 90 revs/min, washing time 12 minutes, control washing water flow 240kg/h, then enter into secondary water-and-oil separator 25 and carry out oily water separation, lower floor's washing soln is driven into one-stage water wash still 21 through secondary water washing cycles pump 26, and the washing water after secondary washing are used as one-level washing water and use; Upper materials component is delivered to tertiary effluent and washes still 27.
Hydrolysate enters tertiary effluent and washes still 27 and clean, washing kettle adopts frame type stirring, stirring velocity 90 revs/min, washing time 12 minutes, control washing water flow 240kg/h, then enter into three grades of water-and-oil separators 28 and carry out oily water separation, lower floor's washing soln through tertiary effluent wash recycle pump 29 be driven into secondary washing kettle 24, three grades washing after washing water be used as secondary washing water use; Upper materials component is delivered to hydrolyzate storage tank 31.
After washing terminates, to realize water-and-oil separator interface by interface automatic control technology constant, thus realize being separated of washing water and oily matter.
C, concentrated and polycondensation
Hydrolysate is delivered to concentrated polycondensation vessel 32 from hydrolyzate storage tank 31, continuous concentration is carried out under vacuum tightness 0 ~ 0.098MPa, deviate from solvent, solvent is delivered to solvent recovery tank 33 through solvent cooler 34, recovered solvent is delivered to distillation purification workshop section through solvent delivery pump 35, and the solvent after purification can be recycled and reused for hydrolysis system.
When material reaches 60% of still volume in polycondensation vessel 32 to be concentrated, carry out polycondensation, add zinc octoate, add that quality is hydrolyzate quality 4 ‰ of zinc octoate, polycondensation temperature is 130 DEG C, and vacuum tightness is 0.075Mpa, grid agitator stirring velocity is 90 revs/min, reacts 4 hours.
When carrying out polycondensation, open vacuum pump, open nitrogen bubble device at the bottom of concentrated polycondensation vessel 32 still, by the stirring of nitrogen with take effect out of, improve low molecular deviate from degree, shorten the de-low time, because a small amount of nitrogen intake just can play the effect of bubbling, so blast nitrogen not affect vacuum.
Add xylene solvent to above-mentioned material effective content mass ratio after polycondensation completes and reach 50%, pack after filtration, obtained silicone resin finished product.
Embodiment 4
A continuous environment-friendly preparation process for high-temperature resistant coating methyl phenyl silicone resin, carries out as follows:
According to following proportioning raw materials charging:
Phenyl-trichloro-silicane: 37kg/h; Diphenyl dichlorosilane: 10kg/h
METHYL TRICHLORO SILANE: 15kg/h; Dimethyldichlorosilane(DMCS): 15kg/h
Dimethylbenzene: 160kg/h; Diluted acid water: 320kg/h
A, hydrolysis
Raw material is dosed in static mixer according to said ratio, after static mixer 11 tentatively mixing, enters pipe type water solution reactor 12, react with diluted acid water.Diluted acid water to be mass concentration be 1% dilute hydrochloric acid (also can adopt the washing water after one-stage water wash in a still material water washing process).Be 20 DEG C by hydrolysis water cooler 15 controlled hydrolysis temperature, reaction table pressure 0.3MPa in hydrolysis reactor, after charging completes, material is 10 minutes in the hydrolysis system residence time.Heat exchange in hydrolysis water cooler 15 is transported material to by hydrolysis recycle pump 14, then enter into preseparator 13 and carry out pre-separation, again by Pipeline transport in acid separator 16, hydrolysate flows out through acid separator 16 upper outlet, be delivered to one-stage water wash still 21 to wash, stirring velocity 120 revs/min; Acid separator 16 lower floor solution goes out to hydrochloric acid cleaner 17 through separator bottom stream, and solution, after hydrochloric acid cleaner 17 purifies, stores, can be used for other industrial production.
B, washing
Hydrolysate is washed till neutrality through tertiary effluent, and during washing, in still, mixeding liquid temperature controls at 50 DEG C, condition of normal pressure.
Water used in water washing process adopts common process water when the first still, and water is afterwards the washing water (the common process water of the hydromining that last step adds) after next stage washing.
Hydrolysate is introduced into one-stage water wash still 21 and cleans, washing kettle adopts frame type stirring, stirring velocity 120 revs/min, washing time 10 minutes, control washing water flow 320kg/h, then enter into primary oil water separator 22 and carry out oily water separation, lower floor's washing soln is driven into tubular type hydrolysis reactor 12 through one-stage water wash recycle pump 23, and the lower floor's washing soln after one-level washing enters the hydrolysis medium that tubular type hydrolysis reactor 12 reacts as next still; Upper materials component is delivered to secondary washing kettle 24.
Hydrolysate enters secondary washing kettle 24 and cleans, washing kettle adopts frame type stirring, stirring velocity 120 revs/min, washing time 10 minutes, control washing water flow 320kg/h, then enter into secondary water-and-oil separator 25 and carry out oily water separation, lower floor's washing soln is driven into one-stage water wash still 21 through secondary water washing cycles pump 26, and the washing water after secondary washing are used as one-level washing water and use; Upper materials component is delivered to tertiary effluent and washes still 27.
Hydrolysate enters tertiary effluent and washes still 27 and clean, washing kettle adopts frame type stirring, stirring velocity 120 revs/min, washing time 10 minutes, control washing water flow 320kg/h, then enter into three grades of water-and-oil separators 28 and carry out oily water separation, lower floor's washing soln through tertiary effluent wash recycle pump 29 be driven into secondary washing kettle 24, three grades washing after washing water be used as secondary washing water use; Upper materials component is delivered to hydrolyzate storage tank 31.
After washing terminates, to realize water-and-oil separator interface by interface automatic control technology constant, thus realize being separated of washing water and oily matter.
C, concentrated and polycondensation
Hydrolysate is delivered to concentrated polycondensation vessel 32 from hydrolyzate storage tank 31, continuous concentration is carried out under vacuum tightness 0 ~ 0.098MPa, deviate from solvent, solvent is delivered to solvent recovery tank 33 through solvent cooler 34, recovered solvent is delivered to distillation purification workshop section through solvent delivery pump 35, and the solvent after purification can be recycled and reused for hydrolysis system.
When material reaches 60% of still volume in polycondensation vessel 32 to be concentrated, carry out polycondensation, add zinc octoate, add that quality is hydrolyzate quality 1.5 ‰ of zinc octoate, polycondensation temperature is 130 DEG C, and vacuum tightness is 0.060Mpa, grid agitator stirring velocity is 120 revs/min, reacts 3 hours.
When carrying out polycondensation, open vacuum pump, open nitrogen bubble device at the bottom of concentrated polycondensation vessel 32 still, by the stirring of nitrogen with take effect out of, improve low molecular deviate from degree, shorten the de-low time, because a small amount of nitrogen intake just can play the effect of bubbling, so blast nitrogen not affect vacuum.
Add xylene solvent to above-mentioned material effective content mass ratio after polycondensation completes and reach 50%, pack after filtration, obtained silicone resin finished product.
Embodiment 5
A continuous environment-friendly preparation process for high-temperature resistant coating methyl phenyl silicone resin, carries out as follows:
According to following proportioning raw materials charging:
Phenyl-trichloro-silicane: 22kg/h; Diphenyl dichlorosilane: 10kg/h
METHYL TRICHLORO SILANE: 15kg/h; Dimethyldichlorosilane(DMCS): 30kg/h
Dimethylbenzene: 160kg/h; Diluted acid water: 240kg/h
A, hydrolysis
Raw material is dosed in static mixer according to said ratio, after static mixer 11 tentatively mixing, enters pipe type water solution reactor 12, react with diluted acid water.Diluted acid water to be mass concentration be 0.8% dilute hydrochloric acid (also can adopt the washing water after one-stage water wash in a still material water washing process).Be 40 DEG C by hydrolysis water cooler 15 controlled hydrolysis temperature, reaction table pressure 0.4MPa in hydrolysis reactor, after charging completes, material is 8 minutes in the hydrolysis system residence time.Heat exchange in hydrolysis water cooler 15 is transported material to by hydrolysis recycle pump 14, then enter into preseparator 13 and carry out pre-separation, again by Pipeline transport in acid separator 16, hydrolysate flows out through acid separator 16 upper outlet, be delivered to one-stage water wash still 21 to wash, stirring velocity 100 revs/min; Acid separator 16 lower floor solution goes out to hydrochloric acid cleaner 17 through separator bottom stream, and solution, after hydrochloric acid cleaner 17 purifies, stores, can be used for other industrial production.
B, washing
Hydrolysate is washed till neutrality through tertiary effluent, and during washing, in still, mixeding liquid temperature controls at 30 DEG C, condition of normal pressure.
Water used in water washing process adopts common process water when the first still, and water is afterwards the washing water (the common process water of the hydromining that last step adds) after next stage washing.
Hydrolysate is introduced into one-stage water wash still 21 and cleans, washing kettle adopts frame type stirring, stirring velocity 100 revs/min, washing time 12 minutes, control washing water flow 240kg/h, then enter into primary oil water separator 22 and carry out oily water separation, lower floor's washing soln is driven into tubular type hydrolysis reactor 12 through one-stage water wash recycle pump 23, and the lower floor's washing soln after one-level washing enters the hydrolysis medium that tubular type hydrolysis reactor 12 reacts as next still; Upper materials component is delivered to secondary washing kettle 24.
Hydrolysate enters secondary washing kettle 24 and cleans, washing kettle adopts frame type stirring, stirring velocity 100 revs/min, washing time 12 minutes, control washing water flow 240kg/h, then enter into secondary water-and-oil separator 25 and carry out oily water separation, lower floor's washing soln is driven into one-stage water wash still 21 through secondary water washing cycles pump 26, and the washing water after secondary washing are used as one-level washing water and use; Upper materials component is delivered to tertiary effluent and washes still 27.
Hydrolysate enters tertiary effluent and washes still 27 and clean, washing kettle adopts frame type stirring, stirring velocity 100 revs/min, washing time 12 minutes, control washing water flow 240kg/h, then enter into three grades of water-and-oil separators 28 and carry out oily water separation, lower floor's washing soln through tertiary effluent wash recycle pump 29 be driven into secondary washing kettle 24, three grades washing after washing water be used as secondary washing water use; Upper materials component is delivered to hydrolyzate storage tank 31.
After washing terminates, to realize water-and-oil separator interface by interface automatic control technology constant, thus realize being separated of washing water and oily matter.
C, concentrated and polycondensation
Hydrolysate is delivered to concentrated polycondensation vessel 32 from hydrolyzate storage tank 31, continuous concentration is carried out under vacuum tightness 0 ~ 0.098MPa, deviate from solvent, solvent is delivered to solvent recovery tank 33 through solvent cooler 34, recovered solvent is delivered to distillation purification workshop section through solvent delivery pump 35, and the solvent after purification can be recycled and reused for hydrolysis system.
When material reaches 60% of still volume in polycondensation vessel 32 to be concentrated, carry out polycondensation, add isocaprylic acid zinc, add that quality is hydrolyzate quality 2 ‰ of isocaprylic acid zinc, polycondensation temperature is 140 DEG C, and vacuum tightness is 0.050Mpa, grid agitator stirring velocity is 100 revs/min, reacts 3 hours.
When carrying out polycondensation, open vacuum pump, open nitrogen bubble device at the bottom of concentrated polycondensation vessel 32 still, by the stirring of nitrogen with take effect out of, improve low molecular deviate from degree, shorten the de-low time, because a small amount of nitrogen intake just can play the effect of bubbling, so blast nitrogen not affect vacuum.
Add xylene solvent to above-mentioned material effective content mass ratio after polycondensation completes and reach 50%, pack after filtration, obtained silicone resin finished product.
Claims (9)
1. a continuous environment-friendly preparation process for high-temperature resistant coating methyl phenyl silicone resin, carries out as follows:
A, hydrolysis
Phenyl-trichloro-silicane, diphenyl dichlorosilane, METHYL TRICHLORO SILANE, dimethyldichlorosilane(DMCS) 1 ~ 20:1 in mass ratio ~ 10:1 ~ 10:1 ~ 20 mix, the quality of benzene series solvent is 1 ~ 3 times of mixed chlorosilane monomer mass, after enter pipe type water solution reactor and diluted acid water reacts, the quality of diluted acid water is 2 ~ 5 times of mixed chlorosilane monomer mass, hydrolysis temperature is 10 ~ 60 DEG C, hydrolysis gauge pressure 0.3 ~ 0.5MPa, after charging completes, material is 2 ~ 30 minutes in the hydrolysis system residence time;
B, washing
Hydrolyzate is washed to neutrality step by step through more than three grades or three grades, washing temperature 30 ~ 80 DEG C, after three grades of washings, water is used as secondary washing, after secondary washing, water is used as one-level washing, after one-level washing, water enters tubular reactor as hydrolysis medium, and the water consumption that water rinses is added equals the washing water consumption entering tubular type hydrolysis reactor;
C, concentrated and polycondensation
Carry out continuous concentration at vacuum tightness 0 ~ 0.098MPa, when material reaches 50% ~ 60% of still volume in polycondensation vessel to be concentrated, add catalyzer, carry out polycondensation, temperature of reaction 120 ~ 160 DEG C, react 2 ~ 4 hours, open bubbling device bottom concentrated polycondensation vessel, blast rare gas element;
D, detection, filtration, packaging, recycled solvent
Add benzene series solvent after polycondensation completes and reach 50% to the said products effective content mass ratio, pack after filtration, become silicone resin finished product.
2. the continuous environment-friendly preparation process of a kind of high-temperature resistant coating methyl phenyl silicone resin according to claim 1, it is characterized in that, in step a diluted acid water to be mass concentration when quantity-produced the first still be 0.9% dilute hydrochloric acid, diluted acid water selected is afterwards the washing water in a upper still water washing process after one-stage water wash.
3. the continuous environment-friendly preparation process of a kind of high-temperature resistant coating methyl phenyl silicone resin according to claim 1, it is characterized in that, in step a, benzene series solvent is dimethylbenzene.
4. the continuous environment-friendly preparation process of a kind of high-temperature resistant coating methyl phenyl silicone resin according to claim 1, it is characterized in that, water washing process processing condition in step b: condition of normal pressure, washing kettle adopts frame type stirring, stirring velocity 80 ~ 120 revs/min, washing time at different levels is 8 ~ 12 minutes.
5. the continuous environment-friendly preparation process of a kind of high-temperature resistant coating methyl phenyl silicone resin according to claim 1, is characterized in that, adopt frame type stirring in step c, stirring velocity 80 ~ 120 revs/min.
6. the continuous environment-friendly preparation process of a kind of high-temperature resistant coating methyl phenyl silicone resin according to claim 1, it is characterized in that, catalyzer used in step c is naphthenate or the octylate of metallic zinc, be naphthalene acid zinc, zinc octoate, isocaprylic acid zinc one of them.
7. the continuous environment-friendly preparation process of a kind of high-temperature resistant coating methyl phenyl silicone resin according to claim 1, it is characterized in that, in step c, the add-on of catalyzer is 0.5 ~ 5 ‰ of hydrolyzate quality.
8. the continuous environment-friendly preparation process of a kind of high-temperature resistant coating methyl phenyl silicone resin according to claim 1, it is characterized in that, the rare gas element described in step c is nitrogen.
9. the continuous environment-friendly preparation process of a kind of high-temperature resistant coating methyl phenyl silicone resin according to claim 1, it is characterized in that, when carrying out polycondensation in step c, vacuum tightness is 0 ~ 0.098MPa.
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Address after: 063305 Nanpu Development Zone, Hebei, Tangshan City Patentee after: Tangshan Sanyou Silicon Industry Co.,Ltd. Address before: 063305 Nanpu Development Zone, Hebei, Tangshan City Patentee before: SANYOU SILICON INDUSTRY Co.,Ltd. |