CN102070489B - Device and method for continuous cyanidation reaction in benzyl cyanide production - Google Patents
Device and method for continuous cyanidation reaction in benzyl cyanide production Download PDFInfo
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- CN102070489B CN102070489B CN201110020822.2A CN201110020822A CN102070489B CN 102070489 B CN102070489 B CN 102070489B CN 201110020822 A CN201110020822 A CN 201110020822A CN 102070489 B CN102070489 B CN 102070489B
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- cyanide
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 27
- SUSQOBVLVYHIEX-UHFFFAOYSA-N phenylacetonitrile Chemical compound N#CCC1=CC=CC=C1 SUSQOBVLVYHIEX-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims abstract description 8
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229940073608 benzyl chloride Drugs 0.000 claims abstract description 13
- 239000012043 crude product Substances 0.000 claims abstract description 11
- 238000000605 extraction Methods 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 239000012295 chemical reaction liquid Substances 0.000 abstract 2
- 239000010779 crude oil Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- 239000002351 wastewater Substances 0.000 description 7
- 238000003860 storage Methods 0.000 description 6
- 239000000945 filler Substances 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 3
- 210000003298 dental enamel Anatomy 0.000 description 3
- 238000010923 batch production Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention discloses a device and a method for continuous cyanidation reaction in benzyl cyanide production, wherein the device comprises a plurality of reaction kettles which are used in series, the reaction kettles are connected through an overflow pipe, benzyl chloride, sodium cyanide and a catalyst are added into a first reaction kettle according to the flow of 0.8-1.6 t/h of benzyl chloride, 1.05-2.1 t/h of sodium cyanide solution and 10-30 l/h of catalyst, the temperature of the first reaction kettle is controlled to be 80-90 ℃, then reaction liquid is subjected to overflow reaction of the plurality of reaction kettles, and finally the reaction liquid enters a settling tank for automatic settling separation, and oil and water are continuously extracted to obtain crude oil. The technology of the invention can ensure that the benzyl cyanide production is continuously and stably operated, the capacity of the device is greatly improved, and the labor intensity of workers is greatly reduced. Meanwhile, the reaction is easy to control, the yield is high, the yield is 98-99%, and the purity of a crude product is 97.0-98.5%.
Description
Technical field
The present invention relates to a kind of apparatus and method of continuous cyanogenation, belong to synthesis technology field.
Background technology
In benzyl cyanide production process, Benzyl Chloride and sodium cyanide react and obtain under the condition of catalyzer existence at present, and cyanogenation is batch production.Batch production is easily rushed material, and dangerous large, labor strength is large.Successive reaction efficiency is high and successive reaction is wayward.Existing reaction unit, feeds in raw material, is incubated, to turn the non-cutting times such as material long, and operation elasticity is little, and reaction temperature control narrow range, is difficult to control poor stability.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, and the apparatus and method of continuous cyanogenation in a kind of benzyl cyanide production are provided.
The technical scheme that the present invention takes is:
The device of continuous cyanogenation in benzyl cyanide production, comprise the reactor that many series connection are used, between reactor, by upflow tube, connect, on First reactor, establish charging opening, a middle reactor is established filler, and last reactor connects subsider by transfering material pump.
Described subsider bottom connects wastewater storage tank by U-shaped bend pipe, and subsider top connects benzyl cyanide crude product storage tank.
Described reactor is five series connection preferably, on the 3rd reactor, establish filler.
The method of continuous cyanogenation in benzyl cyanide production, Benzyl Chloride, sodium cyanide and catalyzer are added to First reactor by the flow of Benzyl Chloride 0.8～1.6t/h, sodium cyanide solution 1.05～2.1t/h, catalyzer 10～30l/h, control 80～90 ℃ of First temperature of reaction kettle, then reaction solution is through the overflow reaction of many reactors, finally entering subsider automatic sedimentation separates, oil and the continuous extraction of water, obtain crude product oil.
At the bottom of subsider, mouth production is waste water, and subsider production suitable for reading is crude product oil.
Described sodium cyanide solution concentration is 30% (wt%), and described catalyzer is the liquid catalyst that cyanogenation is conventional.
It is 40～50 ℃ that last temperature of reaction is reacted in described overflow, and middle several temperature of reaction are 90～95 ℃.
In described overflow reaction, need to add water, amount of water 0.8～1.6t/h.
Above-mentioned flow can with the size of reactor be 3000l～5000l.
The technology of the present invention, can make benzyl cyanide produce continuous and steady operation, and device capability significantly improves, and labor strength reduces greatly.Simultaneous reactions is easy to control, and productive rate is high, productive rate 98～99%, crude product purity 97.0%～98.5%.
Accompanying drawing explanation
Fig. 1 is structure drawing of device of the present invention,
Wherein: 1 is 1# reactor (being main reaction still), 2 is 2# reactor (being secondary reacting kettle), 3 is 3# reactor (adding water still), 4 is 4# reactor (strengthening reactor), and 5 is 5# reactor (still of lowering the temperature), and 6,7,8 is charging opening, 9 is filler, 10 is subsider, and 11 is wastewater storage tank, and 12 is benzyl cyanide crude product storage tank.
Embodiment
The device of continuous cyanogenation in benzyl cyanide production, comprise the reactor that many series connection are used, between reactor, by upflow tube, connect, on First reactor, establish charging opening, a middle reactor is established filler, last reactor connects subsider by transfering material pump, and subsider bottom connects wastewater storage tank by U-shaped bend pipe, and subsider top connects benzyl cyanide crude product storage tank.
Embodiment 1
Adopt 5 3000L enamel stills as reactor, series connection is used, and upflow tube is installed in every still.In First reactor, by Benzyl Chloride 0.8t/h, 30% (wt%) sodium cyanide solution 1.05t/h, catalyzer 10l/h flow, drip continuously Benzyl Chloride, sodium cyanide and catalyzer, then material is entered in 2#, 3#, 4#, 5# reactor successively by the upflow tube of First reactor bottom, by cooling water control still temperature, be respectively 80 ℃, 90 ℃, 90 ℃, 90 ℃, 40 ℃ and stablize, in 3# reactor, by 0.8t/h flow, add continuously water one time.Material in last 5# reactor, as benzyl cyanide crude product, continues to proceed to subsider by transfering material pump and divides water, and subsider wastewater discharge pipe is installed U-shaped curved, makes continuously extraction of You Heshui.Realized the serialization of cyanogenation.
Adopt 5 5000L enamel stills as reactor, series connection is used, and upflow tube is installed in every still.In First still, press Benzyl Chloride 1.6t/h; 30% (wt%) sodium cyanide solution 2.1t/h; Catalyzer 30l/h flow drips Benzyl Chloride, sodium cyanide and catalyzer continuously,
Then material is entered in 2#, 3#, 4#, 5# reactor successively by the upflow tube of First reactor bottom, by cooling water control still temperature, be respectively 90 ℃, 95 ℃, 95 ℃, 95 ℃, 50 ℃ and stablize, in 3# reactor, by 1.6t/h flow, add continuously water one time.Material in last 5# reactor, as benzyl cyanide crude product, continues to proceed to subsider by transfering material pump and divides water, and subsider wastewater discharge pipe is installed U-shaped curved, makes continuously extraction of You Heshui.Realized the serialization of cyanogenation.
Adopt 5 5000L enamel stills as reactor, series connection is used, and upflow tube is installed in every still.In First still, press Benzyl Chloride 1.2t/h; 30% (wt%) sodium cyanide solution 1.6t/h; Catalyzer 20l/h flow drips Benzyl Chloride, sodium cyanide and catalyzer continuously, then material is entered in 2#, 3#, 4#, 5# reactor successively by the upflow tube of First reactor bottom, by cooling water control still temperature, be respectively 85 ℃, 92 ℃, 92 ℃, 92 ℃, 45 ℃ and stablize, in 3# reactor, by 1.3t/h flow, add continuously water one time.Material in last 5# reactor, as benzyl cyanide crude product, continues to proceed to subsider by transfering material pump and divides water, and subsider wastewater discharge pipe is installed U-shaped curved, makes continuously extraction of You Heshui.Realized the serialization of cyanogenation.
Claims (2)
1. the method for continuous cyanogenation in benzyl cyanide production, it is characterized in that, Benzyl Chloride, sodium cyanide and catalyzer are added to First reactor by the flow of Benzyl Chloride 0.8～1.6t/h, sodium cyanide solution 1.05～2.1t/h, catalyzer 10～30l/h, control 80～90 ℃ of First temperature of reaction kettle, then reaction solution is through the overflow reaction of many reactors, finally enter subsider automatic sedimentation and separate, oil and the continuous extraction of water, obtain crude product oil; It is 40～50 ℃ that last temperature of reaction is reacted in described overflow, and middle several temperature of reaction are 90～95 ℃, in described overflow reaction, needs to add water, amount of water 0.8～1.6t/h, and the size of the reactor that described flow is used is 3000l～5000l.
2. the method for continuous cyanogenation in benzyl cyanide production according to claim 1, is characterized in that, described sodium cyanide solution concentration is 30%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110020822.2A CN102070489B (en) | 2011-01-18 | 2011-01-18 | Device and method for continuous cyanidation reaction in benzyl cyanide production |
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| CN201110020822.2A CN102070489B (en) | 2011-01-18 | 2011-01-18 | Device and method for continuous cyanidation reaction in benzyl cyanide production |
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| CN102070489B true CN102070489B (en) | 2014-04-23 |
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| CN105218401B (en) * | 2015-09-21 | 2017-08-11 | 河北诚信有限责任公司 | The method that continuity method synthesizes benzene acetonitrile |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6846946B2 (en) * | 2002-02-15 | 2005-01-25 | Value Recovery, Inc. | Process for making organic products and improving the quality of non-product streams using phase transfer catalysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6846946B2 (en) * | 2002-02-15 | 2005-01-25 | Value Recovery, Inc. | Process for making organic products and improving the quality of non-product streams using phase transfer catalysis |
Non-Patent Citations (2)
| Title |
|---|
| 陆庆松.高纯度苯乙腈合成.《浙江化工》.2001,第32卷(第3期),31-33. |
| 高纯度苯乙腈合成;陆庆松;《浙江化工》;20011231;第32卷(第3期);31-33 * |
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Inventor after: Chen Yunfeng Inventor after: Wu Xianqing Inventor after: Liu Weining Inventor before: Wu Xianqing Inventor before: Liu Weining |
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Address after: 252211 Shandong Liaocheng High-tech Industrial Development Zone Luxi Industrial Park Patentee after: Liaocheng Luxi Chlorobenzyl Chemical Co., Ltd. Address before: 252211 Shandong city of Liaocheng province Dong'e County Gu Luxi Industrial Park Town Patentee before: Shandong Liaocheng Zhongsheng Lanrui Chemical Industry Co., Ltd. |
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Effective date of registration: 20220524 Address after: 252211 new chemical materials Industrial Park, Liaocheng high tech Industrial Development Zone, Shandong Province Patentee after: CHLOR-ALKALI CHEMICAL BRANCH OF LUXI CHEMICAL GROUP Co.,Ltd. Address before: 252211 Shandong Liaocheng High-tech Industrial Development Zone Luxi Industrial Park Patentee before: Liaocheng Luxi Chlorobenzyl Chemical Co.,Ltd. |