CN104277067A - Device and method for reducing chlorine ion content in dimethyldichlorosilance hydrolysate - Google Patents
Device and method for reducing chlorine ion content in dimethyldichlorosilance hydrolysate Download PDFInfo
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- CN104277067A CN104277067A CN201410480225.1A CN201410480225A CN104277067A CN 104277067 A CN104277067 A CN 104277067A CN 201410480225 A CN201410480225 A CN 201410480225A CN 104277067 A CN104277067 A CN 104277067A
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Abstract
The invention discloses a device and a method for reducing chlorine ion content in dimethyldichlorosilance hydrolysate. The device comprises a dechlorinating device, a pressurized circulating pump and a separator, wherein the bottom side part of the dechlorinating device is connected with a water replenishing pipeline and a hydrolysate conveying pipeline; an inlet of the pressurized circulating pump is connected with a storage groove; an outlet is connected with the bottom of the dechlorinating device; the inlet of the side part of the separator is connected with a dechlorinating device outlet pipeline through a pipeline; the top of the separator is connected with a hydrolysate delivery pipeline; the bottom of the separator is connected with a washing water delivery pipeline; and a separator inlet pipeline is connected with a pressure delivery pump outlet pipeline. By adoption of a mixing component, two incompatible mediums such as hydrolysate and washing water can be fully mixed, so that chlorine ions in hydrolysate oil can relatively easily contact with washing water, thus the washing effect is increased, the effect of removing chlorine ions from the hydrolysate oil is achieved, and from the micro view, an oil-water mixed state belongs to the micron scale; therefore, the contact probability of oil and water can be greatly increased, and the reaction and mass transfer efficiency is improved.
Description
Technical field
The present invention relates to organosilicon industry and prepare silicone technology, especially a kind of device and method reducing chloride ion content in Dimethyldichlorosilane hydrolysate.
Background technology
The method reducing residual chlorine ion content in Dimethyldichlorosilane hydrolysate in organosilicon industry mainly contains alkali neutralisation, steam treatment method and adsorption treatment method etc.At present, method the most frequently used is both at home and abroad alkali neutralisation, its technique content is: in thick for dimethyldichlorosilane(DMCS) hydrolyzate and the alkali lye being heated to certain temperature being added continuously by a certain percentage and in still, the residual chlorine in hydrolyzate and alkali is under agitation made to carry out neutralization reaction, thus reducing the content of residual chlorine, after neutralization, hydrolyzate and buck realize layering under gravity; This kind of technique, the mixing quality of oil phase and aqueous phase directly affects neutralization, and the method that there is no at present ensures oil, being uniformly distributed of aqueous phase, and obtains homogeneous phase liquid/liquid mixture, and wastewater discharge is large, meanwhile, cannot to ensure in hydrolyzate not saliferous.In view of the shortcoming of alkali neutralisation, foreign study goes out steam treatment method, its technique is: make the thick hydrolyzate of diformazan enter packed tower or stripping tower from tower top, the water vapour counter current contact of 110-160 DEG C that passes into tower bottom, the siloxanes that tower top and tower reactor obtained merges, for the tower top charging of next tower or with in alkali and; The shortcoming of the method is: owing to adopting high-temperature operation, is difficult to viscosity that is stable and control diformazan hydrolyzate.Another kind method is absorption method, acid aqueous phase is isolated by porous material (as precipitated silica, glass fibre etc.) by hydrolyzate, obtain the hydrolyzate that residual chlorine is lower, but adopt this method may introduce some mechanical impuritys that cannot remove, and in serialization, there is certain problem.Propose in patent documentation 103429602A and use anionite-exchange resin to carry out absorption dechlorination technology, through understanding and experimental demonstration, dechlorination effect is better, but resin regeneration working cost is higher.
Summary of the invention
The object of the invention is, for overcoming above-mentioned the deficiencies in the prior art, a kind of device and method reducing chloride ion content in Dimethyldichlorosilane hydrolysate to be provided, not only to improve the quality of hydrolyzate, decrease wastewater treatment capacity simultaneously.
For achieving the above object, the present invention adopts following technical proposals:
A kind of device reducing chloride ion content in Dimethyldichlorosilane hydrolysate, comprise chlorine purifier, pressurized circulation pump and separator, wherein, described chlorine purifier bottom side and water pipe, conveying hydrolyzate pipeline is connected, described pressurized circulation pump inlet is connected with storage tank by pipeline, described pressurized circulation pump discharge is connected with bottom chlorine purifier by pipeline, described separator side inlet is connected with chlorine purifier export pipeline by pipeline, described separator top with send hydrolyzate pipeline outside and be connected, described separator bottom with send washing water pipeline outside and be connected, described separator interior loads acid corrosion-resistant internals and packing layer.
Described de-salted water refers to that residue saltiness is wherein 1 ~ 5 mg/litre by the contained strong electrolyte removing being easy to remove or the water reduced to a certain degree.
Described water pipe and conveying hydrolyzate pipeline are positioned at the homonymy of chlorine purifier, and water pipe is positioned at the upside of conveying hydrolyzate pipeline.
Built-in micropore in described acid corrosion-resistant internals.
Described packing layer is tensio-active agent.
Described conveying hydrolyzate pipeline is provided with under meter and hydrolyzate pipe-line control valve successively.
Described water pipe is provided with successively under meter and water pipe control valve.
The pipeline that described positive delivery pump discharge is connected with the import of chlorine purifier device bottom is provided with under meter and pipe-line control valve successively.
Present invention also offers a kind of method utilizing said apparatus to reduce chloride ion content in Dimethyldichlorosilane hydrolysate, method is: by Dimethyldichlorosilane hydrolysate and de-salted water respectively through conveying hydrolyzate pipeline, water pipe enters chlorine purifier, according to volume ratio (1-8): the ratio mixing of 1, wash, obtain mixed solution, a part enters storage tank, a part enters separator and carries out oily water separation, in storage tank, mixed solution reenters chlorine purifier circulation cleaning through circulation force (forcing) pump, after separator is separated, send the chloride ion content of the dimethyldichlorosilane(DMCS) in hydrolyzate pipeline outside lower than 3ppm.
The time 10-30min of described hydrolyzate mixing, washing in chlorine purifier.
Described wash temperature is 70-80 DEG C.
The invention has the beneficial effects as follows,
1. the application adopts chlorine purifier and corrosion-resistant internals to enable hydrolyzate and washing water two kinds of mutual exclusive media reach abundant mixing according to a certain percentage, thus make the chlorion in hydrolyzate oil be more prone to contact with washing water, increase washing effect, reach the effect removing chlorion in hydrolyzate oil, from microcosmic angle, oil mixing with water state belongs to micron-sized, thus greatly can increase the probability of oil water contact, improves reaction mass transfer efficiency;
2. the method for the application, can effectively reduce chloride ion content in hydrolyzate siloxanes; And the washing water yield can be reduced; Because chloride ion content reduces, the consumption of the auxiliary material potassium hydroxide of follow-up system cracking unit can be reduced, and the quality of product DMC can be improved, improve the market competitiveness.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Wherein 1. water pipes, 2. carry hydrolyzate pipeline, 3. chlorine purifier, 4. pressurized circulation pump, 5. separator, 6. send hydrolyzate pipeline outside, 7. sends washing water pipeline outside, 8. storage tank.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described.
Embodiment 1:
A kind of device reducing chloride ion content in Dimethyldichlorosilane hydrolysate, comprise chlorine purifier 3, pressurized circulation pump 4 be separated 5 devices, wherein, described chlorine purifier 3 bottom side and water pipe 1, conveying hydrolyzate pipeline 2 is connected, the import of described pressurized circulation pump 4 is connected with storage tank 8 by pipeline, described pressurized circulation pump 4 is exported and is connected with bottom chlorine purifier 3 by pipeline, described separator 5 side inlet is connected with chlorine purifier 3 export pipeline by pipeline, described separator 5 top with send hydrolyzate pipeline 6 outside and be connected, bottom described separator 5 with send washing water pipeline 7 outside and be connected, acid corrosion-resistant internals and packing layer are loaded in described separator 5 inside.
Described water pipe 1 and conveying hydrolyzate pipeline 2 are positioned at the homonymy of chlorine purifier 3, and water pipe 1 is positioned at the upside of conveying hydrolyzate pipeline 2.
Built-in micropore in described acid corrosion-resistant internals.
Described packing layer is tensio-active agent.
Described conveying hydrolyzate pipeline 2 is provided with under meter and hydrolyzate pipe-line control valve successively.
Described water pipe 1 is provided with successively under meter and water pipe control valve.
Described positive delivery pump 4 exports on the pipeline that is connected with the import of chlorine purifier 3 device bottom and is provided with under meter and pipe-line control valve successively.
By 2L dimethyl siloxane hydrolyzate and 2L the de-salted water after heating respectively through carrying hydrolyzate pipeline 2, water pipe 1 enters chlorine purifier 3 continuously, wash, obtain mixed solution, washing temperature controls at 70 DEG C, after circulation cleaning after 30 minutes, a part enters storage tank 8, a part enters separator 5 and carries out oily water separation, after separator 5 is separated, send the chloride ion content of the dimethyldichlorosilane(DMCS) in hydrolyzate pipeline 6 outside through measuring, chloride content is reduced to 2.1ppm by original 15.3ppm.
Embodiment 2:
Reduce a device for chloride ion content in Dimethyldichlorosilane hydrolysate, with embodiment 1.
By 4L dimethyl siloxane hydrolyzate and 2L the de-salted water after heating respectively through carrying hydrolyzate pipeline 2, water pipe 1 enters chlorine purifier 3 continuously, wash, obtain mixed solution, washing temperature controls at 75 DEG C, after circulation cleaning after 20 minutes, a part enters storage tank 8, a part enters separator 5 and carries out oily water separation, after separator 5 is separated, send the chloride ion content of the dimethyldichlorosilane(DMCS) in hydrolyzate pipeline 6 outside through measuring, chloride content is reduced to 2.3ppm by original 15.3ppm.
Embodiment 3:
Reduce a device for chloride ion content in Dimethyldichlorosilane hydrolysate, with embodiment 1.
By 10L dimethyl siloxane hydrolyzate and 2L the de-salted water after heating respectively through carrying hydrolyzate pipeline 2, water pipe 1 enters chlorine purifier 3 continuously, wash, obtain mixed solution, washing temperature controls at 80 DEG C, after circulation cleaning after 10 minutes, a part enters storage tank 8, a part enters separator 5 and carries out oily water separation, after separator 5 is separated, send the chloride ion content of the dimethyldichlorosilane(DMCS) in hydrolyzate pipeline 6 outside through measuring, chloride content is reduced to 2.5ppm by original 15.3ppm.
Example 4:
Reduce a device for chloride ion content in Dimethyldichlorosilane hydrolysate, with embodiment 1.
By 16L dimethyl siloxane hydrolyzate and 2L the de-salted water after heating respectively through carrying hydrolyzate pipeline 2, water pipe 1 enters chlorine purifier 3 continuously, wash, obtain mixed solution, washing temperature controls at 70 DEG C, after circulation cleaning after 10 minutes, a part enters storage tank 8, a part enters separator 5 and carries out oily water separation, after separator 5 is separated, send the chloride ion content of the dimethyldichlorosilane(DMCS) in hydrolyzate pipeline 6 outside through measuring, chloride content is reduced to 2.9ppm by original 15.3ppm.
Table 1 embodiment 1-4 result table
Reached a conclusion by above case, adopt this method, under the normal production control index of guarantee and thick hydrolyzate and de-salted water ratio situation, the product hydrolysis thing chloride ion content finally obtained can control completely at below 3ppm, meet the demand on producing, meanwhile, decrease the energy consumption that washing water consumption not only effectively reduces unit product, decrease wastewater treatment capacity.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (10)
1. one kind is reduced the device of chloride ion content in Dimethyldichlorosilane hydrolysate, it is characterized in that, comprise chlorine purifier, pressurized circulation pump and separator, wherein, described chlorine purifier bottom side and water pipe, conveying hydrolyzate pipeline is connected, described pressurized circulation pump inlet is connected with storage tank by pipeline, described pressurized circulation pump discharge is connected with bottom chlorine purifier by pipeline, described separator side inlet is connected with chlorine purifier export pipeline by pipeline, described separator top with send hydrolyzate pipeline outside and be connected, described separator bottom with send washing water pipeline outside and be connected, described separator interior loads acid corrosion-resistant internals and packing layer.
2. a kind of device reducing chloride ion content in Dimethyldichlorosilane hydrolysate as claimed in claim 1, is characterized in that, described water pipe and conveying hydrolyzate pipeline are positioned at the homonymy of chlorine purifier, and water pipe is positioned at the upside of conveying hydrolyzate pipeline.
3. a kind of device reducing chloride ion content in Dimethyldichlorosilane hydrolysate as claimed in claim 1, is characterized in that, built-in micropore in described acid corrosion-resistant internals.
4. a kind of device reducing chloride ion content in Dimethyldichlorosilane hydrolysate as claimed in claim 1, is characterized in that, described packing layer is tensio-active agent.
5. a kind of device reducing chloride ion content in Dimethyldichlorosilane hydrolysate as claimed in claim 1, is characterized in that, described conveying hydrolyzate pipeline is provided with under meter and hydrolyzate pipe-line control valve successively.
6. a kind of device reducing chloride ion content in Dimethyldichlorosilane hydrolysate as claimed in claim 1, is characterized in that, described water pipe is provided with successively under meter and water pipe control valve.
7. a kind of device reducing chloride ion content in Dimethyldichlorosilane hydrolysate as claimed in claim 1, is characterized in that, the pipeline that described positive delivery pump discharge is connected with the import of chlorine purifier device bottom is provided with under meter and pipe-line control valve successively.
8. the method for chloride ion content in the reduction Dimethyldichlorosilane hydrolysate as described in any one of claim 1-7, it is characterized in that, by Dimethyldichlorosilane hydrolysate and de-salted water respectively through conveying hydrolyzate pipeline, water pipe enters chlorine purifier, according to volume ratio (1-8): the ratio mixing of 1, wash, obtain mixed solution, a part enters storage tank, a part enters separator and carries out oily water separation, in storage tank, mixed solution reenters chlorine purifier circulation cleaning through circulation force (forcing) pump, after separator is separated, send the chloride ion content of the dimethyldichlorosilane(DMCS) in hydrolyzate pipeline outside lower than 3ppm.
9. the method reducing chloride ion content in Dimethyldichlorosilane hydrolysate as claimed in claim 8, is characterized in that, the time 10-30min of described hydrolyzate mixing, washing in chlorine purifier.
10. the method reducing chloride ion content in Dimethyldichlorosilane hydrolysate as claimed in claim 8, it is characterized in that, described wash temperature is 70-80 DEG C.
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Cited By (5)
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| CN110183479A (en) * | 2019-06-17 | 2019-08-30 | 鲁西化工集团股份有限公司 | A kind of system and technique of the hydrolysis of low pressure dimethyldichlorosilane |
| CN110550773A (en) * | 2019-08-16 | 2019-12-10 | 江西蓝星星火有机硅有限公司 | Method and device for reducing content of chloride ions and other impurities in dimethyl dichlorosilane hydrolysate |
| CN113372373A (en) * | 2021-06-09 | 2021-09-10 | 江西蓝星星火有机硅有限公司 | Device and method for purifying hydrolysate of dimethyl hydrochlorosilane |
| CN114516976A (en) * | 2022-01-28 | 2022-05-20 | 云南能投硅材科技发展有限公司 | Dimethyl dichlorosilane hydrolysis waste pretreatment process |
| WO2022213890A1 (en) * | 2021-04-09 | 2022-10-13 | 江西蓝星星火有机硅有限公司 | Process for producing organosilicon linear body |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110183479A (en) * | 2019-06-17 | 2019-08-30 | 鲁西化工集团股份有限公司 | A kind of system and technique of the hydrolysis of low pressure dimethyldichlorosilane |
| CN110550773A (en) * | 2019-08-16 | 2019-12-10 | 江西蓝星星火有机硅有限公司 | Method and device for reducing content of chloride ions and other impurities in dimethyl dichlorosilane hydrolysate |
| WO2022213890A1 (en) * | 2021-04-09 | 2022-10-13 | 江西蓝星星火有机硅有限公司 | Process for producing organosilicon linear body |
| CN113372373A (en) * | 2021-06-09 | 2021-09-10 | 江西蓝星星火有机硅有限公司 | Device and method for purifying hydrolysate of dimethyl hydrochlorosilane |
| CN113372373B (en) * | 2021-06-09 | 2022-05-17 | 江西蓝星星火有机硅有限公司 | Device and method for purifying hydrolysate of dimethyl hydrochlorosilane |
| CN114516976A (en) * | 2022-01-28 | 2022-05-20 | 云南能投硅材科技发展有限公司 | Dimethyl dichlorosilane hydrolysis waste pretreatment process |
| CN114516976B (en) * | 2022-01-28 | 2024-01-12 | 云南能投硅材科技发展有限公司 | Pretreatment process for hydrolysis waste of dimethyl dichlorosilane |
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