CN201591991U - Gamma-chloropropyltrichlorosilane distilling apparatus - Google Patents

Gamma-chloropropyltrichlorosilane distilling apparatus Download PDF

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Publication number
CN201591991U
CN201591991U CN2009202820601U CN200920282060U CN201591991U CN 201591991 U CN201591991 U CN 201591991U CN 2009202820601 U CN2009202820601 U CN 2009202820601U CN 200920282060 U CN200920282060 U CN 200920282060U CN 201591991 U CN201591991 U CN 201591991U
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distilling apparatus
jar
silane
outlet
rectifying still
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Expired - Fee Related
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CN2009202820601U
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Chinese (zh)
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张中法
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Individual
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Individual
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Abstract

The utility model discloses a Gamma-chloropropyltrichlorosilane distilling apparatus. The distilling apparatus consists of a rectifying still, a distillation tower directly connected with the rectifying still, a condenser connected with an outlet of the distillation tower, a secondary distillation tank connected with an outlet of the condenser by a pipeline, a middle distillation tank and a finished product tank, wherein the distilling apparatus also comprises a primary distillation tank; and the primary distillation tank, the secondary distillation tank, the middle distillation tank and the finished product tank are connected with the outlet of the condenser in parallel. In the distilling apparatus used in the production of the Gamma-chloropropyltrichlorosilane, the primary distillation tank is additionally arranged in the original distilling apparatus, and the unreacted raw materials and the transition-state complex generated in the reaction process are separately recycled and utilized, thus reducing the loss of raw materials, reducing the production cost, and improving the main content of other distilling components accordingly.

Description

γ-chloropropyl trichloro-silane distilling apparatus
Technical field
The utility model relates to the chemical industry equipment field, relates in particular to a kind of distilling apparatus in γ-chloropropyl trichloro-silane production.
Background technology
γ-chloropropyl trichloro-silane is the important monomer of synthesizing series silane coupler product, be widely used in industries such as glass, casting, yarn fabric auxiliary agent, insulating materials, adhesive, also be used to produce agricultural chemicals and medicine intermediate, coating, water treatment auxiliary agents etc., development prospect is very wide.
As catalyst, is raw material with trichlorosilane and chloropropene with compound such as platinum, rhodium, palladium or complex compound, and producing γ-chloropropyl trichloro-silanes through processes such as the addition of silicon hydrogen, distillations is comparatively ripe at present technologies.Existing technology exists mainly that product cost height, γ chloropropyl trichloro-silane yield are low, raw material trichlorosilane and problem such as the chloropropene loss amount is big, accessory substance is many, and this product economy benefit is affected.Therefore, except conscientiously research on synthesis technique, select to use appropriate catalyst, co-catalyst and other auxiliary agent, regulate technological parameter, adopt outside the best feed way, distillation process improved recycle the not raw material of complete reaction to greatest extent, reduce the content of raw material in other cut and have the certain economic meaning.
Rectification working process during present γ-chloropropyl trichloro-silane is produced only steams first and second cut mostly in the operation, these several steps of midbarrel and finished product are separated removal process.And this product is longer because of the reaction time, there is side reaction, and reaction not exclusively, so during the reaction end of determining to technology, still there is not a spot of raw material in the reaction system, therefore, exist raw material and first and second cut separating effect bad in traditional rectification process, the big and high problem of cost of significant loss amount.
Summary of the invention
Technical problem to be solved in the utility model provides a kind of γ-chloropropyl trichloro-silane distilling apparatus, improves a raw material and a secondary fraction separation effect in γ-chloropropyl trichloro-silane still-process, reduces the loss of raw material.
For solving the problems of the technologies described above, the technical solution of the utility model is:
γ-chloropropyl trichloro-silane distilling apparatus, described distilling apparatus comprises rectifying still, the secondary distillate drum, midbarrel jar and the finished product jar that are connected by pipeline with the direct-connected destilling tower of described rectifying still, the condenser that is connected with the outlet of described destilling tower, with condensator outlet, described distilling apparatus also comprises the head fraction jar, and described head fraction jar, a secondary distillate drum, midbarrel jar and finished product jar are connected the outlet of described condenser side by side.
Be connected with return line between described rectifying still and the described condensator outlet.
Described head fraction jar is provided with the raw material reclaim line and connects γ-chloropropyl trichloro-silane reactor.
Be connected with intermediate duct between described midbarrel jar and the described rectifying still.
Owing to adopted technique scheme, the beneficial effects of the utility model are:
1, the utility model is set up the head fraction jar in distilling apparatus, the transition state complex compound of unreacted raw material and course of reaction generation is recycled separately, no longer mix recovery with other cut, therefore comparatively complete with other fraction separation, reduced the loss of raw material, reduced production cost, and the corresponding main content that has improved other cut.
2, the utility model is provided with a return line at the condensator outlet place and is connected with rectifying still, by regulating, determining suitable reflux ratio, has guaranteed that target reclaims the higher yield of raw material.
3, the utility model turns back to γ-chloropropyl trichloro-silane reactor with the head fraction that reclaims, and the active component raw material that contains in the head fraction can be made full use of, and causes, promotes reaction to play positive impetus smoothly fast for initial reaction stage.
Description of drawings
Accompanying drawing is a structural representation of the present utility model;
Among the figure, 1. rectifying still; 2. condenser; 3. a secondary distillate drum; 4. midbarrel jar; 5. finished product jar; 6. head fraction jar; 7. return line; 8. intermediate duct; 9. raw material reclaim line; 10. a secondary cut storage tank; 11. finished product storage tank; 12 destilling towers.
The specific embodiment
As shown in drawings, γ-chloropropyl trichloro-silane distilling apparatus, comprise rectifying still 1, with described rectifying still 1 direct-connected destilling tower 12, the condenser 2 that is connected with 12 outlets of described destilling tower, export a secondary distillate drum 3, midbarrel jar 4 and the finished product jar 5 that is connected by pipeline with condenser 2, described distilling apparatus also comprises head fraction jar 6, and described head fraction jar 6 and a secondary distillate drum 3, midbarrel jar 4 and finished product jar 5 are connected in the outlet of condenser 2 side by side.Be connected with return line 7 between rectifying still 1 and 2 outlets of described condenser, head fraction jar 6 is provided with raw material reclaim line 9 and is communicated with γ-chloropropyl trichloro-silane reactor, is connected with intermediate duct 8 between midbarrel jar 4 and the rectifying still 1.The outlet of one secondary distillate drum 3 is communicated with a secondary cut storage tank 10, and the outlet of finished product jar 5 is communicated with finished product storage tank 11.
During the utility model work, after γ-the chloropropyl trichloro-silane reaction kettle for reaction finishes, change reacted mother liquor over to rectifying still 1 and carry out batch fractionating, when temperature in the rectifying still 1 rises to more than 100 ℃, when still top temperature rises to 40 ℃, open the valve on the return line 7, refluxed 30 minutes.Controlling the rectifying still temperature then is 80 ℃~120 ℃, 30 ℃~50 ℃ of top temperature, keep 1: 4 little reflux ratio, discharging flow is not more than 300L/h, the cut that receives is collected head fraction jar 6, and head fraction turns back to γ-chloropropyl trichloro-silane reactor through raw material reclaim line 9 and continues to participate in reaction.
Then, control suitable rectification temperature, gather respectively and reclaim a secondary cut, midbarrel and finished product cut to secondary distillate drum 3, midbarrel jar 4 and finished product jar 5, midbarrel is returned by intermediate duct 8 and is carried out secondary rectifying in the rectifying still 1, one secondary cut removes a secondary cut storage tank 10, and the finished product cut goes finished product storage tank 11.
Because under the normal pressure, the trichlorosilane boiling point is 31.8 ℃, the chloropropene boiling point is 45 ℃, therefore the head fraction that is received mainly is the transition state complex compound of unreacted raw material and catalyst, after head fraction gathered recovery separately, not only reduce the loss of raw material, also improved the main content of other cut simultaneously.

Claims (4)

1. γ-chloropropyl trichloro-silane distilling apparatus, described distilling apparatus comprises rectifying still, the secondary distillate drum, midbarrel jar and the finished product jar that are connected by pipeline with the direct-connected destilling tower of described rectifying still, the condenser that is connected with the outlet of described destilling tower, with condensator outlet, it is characterized in that: described distilling apparatus also comprises the head fraction jar, and described head fraction jar, a secondary distillate drum, midbarrel jar and finished product jar are connected the outlet of described condenser side by side.
2. γ as claimed in claim 1-chloropropyl trichloro-silane distilling apparatus is characterized in that: be connected with return line between described rectifying still and the described condensator outlet.
3. γ as claimed in claim 2-chloropropyl trichloro-silane distilling apparatus is characterized in that: described head fraction jar is provided with the raw material reclaim line and connects γ-chloropropyl trichloro-silane reactor.
4. γ as claimed in claim 3-chloropropyl trichloro-silane distilling apparatus is characterized in that: be connected with intermediate duct between described midbarrel jar and the described rectifying still.
CN2009202820601U 2009-11-24 2009-11-24 Gamma-chloropropyltrichlorosilane distilling apparatus Expired - Fee Related CN201591991U (en)

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Application Number Priority Date Filing Date Title
CN2009202820601U CN201591991U (en) 2009-11-24 2009-11-24 Gamma-chloropropyltrichlorosilane distilling apparatus

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CN201591991U true CN201591991U (en) 2010-09-29

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102127104A (en) * 2010-12-04 2011-07-20 郭学阳 Method for producing gamma-chloropropyl trichlorosilane
CN102580339A (en) * 2012-03-16 2012-07-18 四川新光硅业科技有限责任公司 Internal reflux rectifying device
CN104262384A (en) * 2014-08-21 2015-01-07 爱斯特(成都)生物制药有限公司 Device and method for rectification purification of 3-isocyanatopropyltriethoxysilane
CN112451985A (en) * 2020-12-11 2021-03-09 浙江开化合成材料有限公司 Continuous production device for silane coupling agent

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102127104A (en) * 2010-12-04 2011-07-20 郭学阳 Method for producing gamma-chloropropyl trichlorosilane
CN102127104B (en) * 2010-12-04 2013-07-31 郭学阳 Method for producing gamma-chloropropyl trichlorosilane
CN102580339A (en) * 2012-03-16 2012-07-18 四川新光硅业科技有限责任公司 Internal reflux rectifying device
CN104262384A (en) * 2014-08-21 2015-01-07 爱斯特(成都)生物制药有限公司 Device and method for rectification purification of 3-isocyanatopropyltriethoxysilane
CN112451985A (en) * 2020-12-11 2021-03-09 浙江开化合成材料有限公司 Continuous production device for silane coupling agent

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C17 Cessation of patent right
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Granted publication date: 20100929

Termination date: 20111124